Comparing Microstructures of ITO Sputtering Targets Prepared by Tin Doped Indium Oxide Powders and In2O3- SnO2 Mixed Powders

磁控溅射ITO靶材制备ITO透明导电薄膜作为平板显示、太阳能电池、气敏元件等电子器件的电极材料,需要ITO靶材具有高纯度、高均匀性、高密度、高导电性的特点。对比研究了ITO共沉淀粉与In2O3、SnO2单体混合粉同炉烧结ITO靶材的微观组织结构差异,如：晶粒尺寸分布、晶粒形貌、元素分布、烧结速率等。结果表明：单体混合粉的烧结速率要比共沉淀粉的烧结速率高,但是前者烧结ITO靶材的微观组织结构不及后者烧结的均匀性好。对比而言,共沉淀粉更容易获得结构组织均匀的ITO靶材,但前提是要合理的设计烧结工艺抑制烧结过程中In2O3的分解。研究结果将会对提高ITO靶材微观组织均匀性和减少靶材毒化,进而提高靶材生产效率提供有益的参考     

Fabrication and structure characterization of ITO transparent conducting film by sol-gel technique

Using In（NO3）3·5H2O and acetylacetone as raw materials and anhydrous SnCl4 as dopant, the transparent conducting indium tin oxide（ITO） films were prepared by sol-gel and dip-coating technique. The phase transformation, structure properties and physical properties （sheet resistance and transmittance） of the films were investigated by DTA-TG, XRD, SEM, four-probe method and UV-Vis spectrometry. The results indicate that it is feasible to fabricate 1TO films on the quartz substrates by sol-gel technique, and the ITO films are formed by accumulating of particles with the size of several decades of nanometers. The prepared ITO film has cubic bixbyite structure, and （111） is its preferred plane. After five-times dip-coating, the 1TO film has a thickness less than 150 nm, a sheet resistance of 110Ω/□, a resistivity of 1.65×10^-3Ω· cm and a transparency of 90% .     

高迁移率的钛掺杂氧化铟薄膜在晶硅/非晶硅异质结电池上的应用研究

采用钛掺杂氧化铟旋转靶制备透明导电薄膜应用在晶硅/非晶硅异质结电池上。在不同氧含量下,研究钛掺杂氧化铟薄膜(T100薄膜)的光电性能,同时对比分析ITO薄膜。在电镜下T100薄膜呈现出柱状结构,并且展示出优异的光学性能。T100薄膜最大载流子迁移率可以达到75.6 cm~2·(V·s)^-1。相比于ITO薄膜,T100薄膜具有优异的电学传导和透光率,因此在异质结电池量产线上电池转换效率可以实现0.26%的提升。     

Reactive magnetron sputtering of indium tin oxide films on acrylics—Electrical resistivity and optical properties

The effects of processing parameters on the deposition rate lattice parameters, stoichiometric compositions, surface morphology, and bonding state of indium tin oxide (ITO) films on acrylics had been previously reported. This study was a continuation of the previous investigation and focused on the electrical resistivity and optical properties of ITO films. The electrical resistivity decreased and then increased with oxygen flow rate. This was due to the effects of oxygen vacancies and impurity scattering. The resistivity of ITO films decreased with the applied bias voltage and film thickness. The transmittance of visible light increased with the oxygen flow rate and decreased with film thickness. Films deposited at oxygen flow rates having low electrical resistivity also had higher infrared radiation (IR) reflectance.     

铟在碱性溶液中的阳极钝化过程

用线性电位扫描、循环伏安、计时电量及电位衰减等电化学方法，研究了铟在3mol／L KOH溶液中的阳极钝化过程．铟在强碱性溶液中表现为一种活化一钝化金属．在活化区铟发生两步氧化，首先一电子氧化形成[InOH]ad，接着[InOH]ad二电子氧化成[In(OH)3]ad，较低电位下前者较快后者较慢，表现为一电子反应；较高电位下两者均较快，表现为三电子反应，两者均受扩散步骤控制．单层[In(OH)3]ad形成后使铟进入钝化区，[In(OH)3]ad不稳定，在碱液中可以溶解和转变为In2O3．在钝化区，铟直接氧化成三价铟，较高电位下形成稳定的In2O3，较低电位下形成非化学计量的三价铟氧化物，其稳定性介于[In(OH)3]ad和In2O3之间。     

溶胶凝胶模板法合成ITO纳米管及其氢敏性能

采用简单的溶胶凝胶阳极氧化铝模板法制备了ITO纳米管.通过FE-SEM、HRTEM、XRD对其微观形貌、结构、相组成等进行了表征和分析,并测试了其对H_2的气敏特性.结果表明,所得纳米管是由10～20 nm晶粒组成的多晶结构,壁厚约为25 nm,平均直径约250 nm,与AAO (Anodic Aluminum Oxide)模板的直径相同.产物在550 ℃热处理后为立方铁锰矿结构的In_2O_3,Sn~(4+)已经掺杂到In_2O_3的晶格中.所得ITO纳米管常温下对氢气具有较好的敏感性及稳定性.     

Synthesis and sintering of indium tin oxide nanoparticles by citrate-nitrate combustion method

Spherical indium tin oxide(ITO) nanoparticles were synthesized by combustion method using citric acid as fuel and nitrates as oxidizer.The obtained ITO nanoparticles were characterized by TG-DSC,FT-IR,XRD,BET,TEM,and SEM.The ITO nanoparticles grew steadily with the increase of heat treatment temperature,and the 700℃ calcined particles had a crystallite size of 25.3 nm and a specific surface area of 26.1 m2·g-1.The avoidance of chlorine ions in the synthesis process decreases particle agglomeration and promotes powder densification.The 900℃ sintered pellet had a density of 67.6% of theoretical density(TD) and increased steadily to 97.3% for the 1400℃ sintered ceramics,respectively.     

In2O3对Ni60激光熔覆层的影响

向Ni60合金粉末中加入适量的In2O3选取合适的工艺参数，采用激光熔覆技术在45钢表面上获得了无裂纹的高质量熔覆层。对熔覆层显微组织进行了观察和分析，测试了熔覆层的显微硬度和摩擦磨损性能。结果表明，同未加入In2O3的Ni60激光熔覆层相比，加入适当比例In2O3的Ni60熔覆层，虽然硬度有所降低，但硬度分布更加均匀，且在该文摩擦条件下耐磨性提高。In2O3能够降低Ni60激光熔覆层裂纹敏感性的原因在于适量的In2O3能够抑制粗大块状硬质相的生长，改善枝晶分布，细化组织晶粒，提高涂层韧性。     

Effect of Sn~(4+) content on properties of indium tin oxide nanopowders

Indium tin oxide(ITO)nanopowders were prepared by a modified chemical co-precipitation process.The influence of different SnO2 contents on the decomposition behavior of ITO precursors,and on the phase and morphology of ITO precursors and ITO nanopowders were studied by X-ray diffractometry,transmission electron microscopy and differential thermal and thermogravimetry analysis methods.The TG-DSC curves show that the decomposition process of precursor precipitation is completed when the temperature is close to 600 ℃and the end temperature of decompositionis somewhat lower when the doping amount of SnO2 is increased.The XRD patterns indicate that the solubility limit of Sn4+ relates directly to the calcining temperature. When being calcined at 700℃,a single phase ITO powder with 15%SnO2(mass fraction)can be obtained.But,when the calcining temperature is higher than 800℃,the phase of SnO2 will appear in ITO nanopowders which contain more than 10%SnO2.The particle size of the ITO nanopowders is 15-25 nm.The ITO nanoparticles without Sn have a spherical shape,but their morphology moves towards an irregular shape when being doped with Sn4+.     

Influence of temperature and layers on the characterization of ITO films

In this paper, the effects of high heating temperature on electrical and optical properties of transparent indium tin oxide (ITO) films were investigated, which is a topic that has received little attention from previous studies. Uniform and transparent indium tin oxide (ITO) films were deposited onto quartz glass substrates through a sol–gel process. Specifically, the microstructure and phase of the films were analyzed by AFM, AES, and XRD. The sheet resistance and optical transmittance of the films were measured using the four-point probe method and spectrophotometer, respectively. The grain size of the ITO film was refined when it heated at 800 °C. The influence of coating layers on electrical and optical properties was also discussed. With the rise of heating temperature from 400 to 800 °C, the optical transmittance of the films climbed from 76 to 93% (750 °C). With the increase of dip-coating layers from 3 to 7, their sheet resistance varied from 642.1 to 241.0 Ω/□.     

Effect of surfactants on the structure and photoelectric properties of ITO films by sol-gel method

The Indium tin oxide(ITO) thin film possesses excellent photoelectric properties that enable it to act as an ideal transparent conductor.To obtain high-quality ITO films through sol-gel method, the ionic surfactant monoethanolamine and the non-ionic surfactant polyethylene glycol(PEG) were added to the ITO precursor slurry.The influences of surfactants on the structural and photoelectric properties of ITO film samples were investigated.XRD patterns indicated that surfactant monoethanolamine contributed to f...     

The characteristics of indium tin oxide films prepared on various buffer layer-coated polymer substrates

The optoelectronic and mechanical properties of flexible indium tin oxide (ITO) films are critical to the development of flexible optoelectronic devices. To improve the characteristics of the flexible films, the effects of inorganic buffer layers on the optoelectronic and mechanical characteristics of flexible ITO films prepared by ion-beam assisted deposition at room temperature were investigated. The results show that four inorganic buffer materials: SiO₂, Ta₂O₅, Al₂O₃ and TiO₂, have different effects on the optical transmission, sheet resistance and mechanical properties of ITO films. Ta₂O₅ buffer layer induces the highest optical transmission. SiO₂ buffer layer leads to the lowest sheet resistance. TiO₂ buffer layer reveals the most superior electrical stability against bending, which is attributed to the low thermal stress in ITO film.     

Microstructure and properties of indium tin oxide thin films deposited by RF-magnetron sputtering

Tin-doped indium oxide （ITO） thin films were prepared using conventional radio frequency （RF） planar magnetron sputtering equipped with IR irradiation using a ceramic target of In2O3/SnO2 with a mass ratio of 1：1 at various IR irradiation temperatures T1 （from room temperature to 400℃）. The refractive index, deposited ratio, and resistivity are functions of the sputtering Ar gas pressure. The microstructure of ITO thin films is related to IR T1, the crystalline seeds appear at T1= 300℃, and the films are amorphous at the temperature ranging from 27℃ to 400℃. AFM investigation shows that the roughness value of peak-valley of ITO thin film （Rp-v） and the surface microstructure of rio thin films have a close relation with T1. The IR irradiation results in a widening value of band-gap energy due to Burstein-Moss effect and the maximum visible transmittance shifts toward a shorter wavelength along with a decrease in the film＇s refractive index. The plasma wavelength and the refractive index of ITO thin films are relative to the T1. XPS investigation shows that the photoelectrolytic properties can be deteriorated by the sub-oxides. The deterioration can be decreased by increasing the oxygen flow rote （fo2）, and the mole ratio of Sn/In in the samples reduces with an increase info2.     

Enrichment by air classification of indium components from In-containing scrap powders scraped by sand-blasting chamber shields of sputter coaters

Raw scrap powders containing 10 wt.% In were recovered by sand-blasting chamber shields of sputter coaters and used as a sole source of indium components for both sieving and air-classification. Sieving was performed first as a feasibility test, and enrichment of indium com-ponent was possible up to 19 wt.% with a mesh size of 635. With this experimental basis, the raw scrap powders were air-classified into 12 lots according to the revolution per minute (r/min) of a single horizontally arranged classifying wheel: 4000, 6000, 8000, 10000, 12000, and 14000 r/min. The particle cut size varied from 56 to 5 μm with turbo wheel speeds corresponding to 4000 to 14000 r/min, respectively, and enrichment of indium component was possible in fine overflow fractions at all turbo wheel speeds while the indium components were not concentrated in all of the coarse underflow fractions. The grade of the indium components became higher with decreasing particle size of the air-classified scrap powders, with the highest grade obtained in the fine overflow fraction with a turbo wheel speed of 14000 r/min. The amount of indium in the fine overflow fractions varied between 15.9 wt.% and 31.5 wt.%. All in all, the grade or purity of the indium com-ponent improved rather significantly from 15.9 wt.% to 31.5 wt.% by air-classification, but this also resulted in overall decrease in recovery rate from 99.33% to 49.64%. Therefore, enrichment and separation of indium should be optimized for maximum recovery and grade of the indium components, which can be used as raw materials in the subsequent electro-refining processes.     

Preparation of silver tin oxide powders by hydrothermal reduction and crystallization

Silver tin oxide composite powders were synthesized by the hydrothermal method with a silver ammine solution and a Na2SnO3 solution as raw materials. H2C2O4 was used as the co-precipitator of silver ions and tin ions. The co-precipitation conditions were investigated. The results show that the co-precipitate of Ag2C2O4 and Sn（OH）4 is available when the pH value of the solution is 4.27-8.36. Using the obtained precipitate as precursor,the reduction of Ag＋ and the crystallization of tin oxide were carried out simultaneously by the hydrothermal method and silver tin oxide composite powders were obtained. The composite powders were characterized by X-ray diffraction （XRD） analysis,scanning electron microscope （SEM）,and energy spectrum analysis. The results show that the silver tin oxide composite powders are small with a diameter of about 2 μm and with homogeneous distribution of tin.     

Preparation of indium tin oxide targets with a high density and single phase structure by normal pressure sintering process

The present work mainly describes the technology for preparing indium-tin oxide (ITO) targets by cold isostatic pressing (CIP) and normal pressure sintering process.ITO powders were produced by chemical co-precipitation and shaped into an ITO green compact with a relative density of 60% by CIP under 300 MPa.Then,an ITO target with a relative density larger than 99.6% was obtained by sintering this green compact at 1550 ℃ for 8 h.The effects of forming pressure,sintering temperature and sintering time on the...     

Influence of Annealing Temperature on the Microstructure and Electrical Properties of Indium Tin Oxide Thin Films

Indium tin oxide(ITO) thin films were prepared on alumina ceramic substrates by radio frequency magnetron sputtering.The samples were subsequently annealed in air at temperatures ranging from 500 to 1,100 °C for 1 h.The influences of the annealing temperature on the microstructure and electrical properties of the ITO thin films were investigated,and the results indicate that the as-deposited ITO thin films are amorphous in nature.All samples were crystallized by annealing at 500 °C.As the annealing temperature increases,the predominant orientation shifts from(222)to(400).The carrier concentration decreases initially and then increases when the annealing temperature rises beyond1,000 °C.The resistivity of the ITO thin films increases smoothly as the annealing temperature increases to just below900 °C.Beyond 900 °C,however,the resistivity of the films increases sharply.The annealing temperature has a significant effect on the stability of the ITO/Pt thin film thermocouples(TFTCs).TFTCs annealed at 1,000 °C show improved hightemperature stability and Seebeck coefficients of up to 77.73 μV/°C.     

氧流量对铟锡氧化物薄膜光电性能的影响

采用射频磁控溅射法，在不同氧流量（0～10sccm）的条件下沉积了铟锡氧化物（In2O3-SnO2）透明导电薄膜。紫外分光光度计测试薄膜的透射率，四点探针测试薄膜的方阻，椭偏仪测试薄膜的复折射率和薄膜厚度，XPS测试ITO薄膜的成分和电子结构。结果表明：薄膜的沉积速率和折射率与氧流量有关，薄膜厚度为60nm，氧流量在9sccm时，透射率超过80％（波长λ=400nm～700nm，包括玻璃基体），退火后透射率、方阻明显改善。XPS分析表明，薄膜中的亚氧化物的存在降低了薄膜的光电性能，控制氧流量可减少亚氧化物。     

Resistive Switching Behavior of Hafnium Oxide Thin Film Grown by Magnetron Sputtering

采用磁控溅射法,以ITO/Glass为衬底,制备了具有电阻转变特性的HfO2薄膜。X射线光电子能谱(XPS)分析发现,薄膜中的Hf、O元素不成化学计量比,薄膜中可能存在大量氧空位。电学测试结果表明,HfO2薄膜表现出明显的双极电阻转变特性,并且表现出良好的可靠性(室温下可重复测试102次以上)和稳定的保持性能(0.5 V偏压下保持104 s以上),高低阻态比值达到104。基于XPS以及电学分析,薄膜的导电过程可用与氧空位相关的空间电荷限制电流模型解释。     

Effects of pretreatment of substrates on the preparation of large scale ZnO nanotube arrays

Well-aligned hexagonal ZnO nanotubes (NTs) arrays were synthesized on pretreated indium fin oxide (ITO) substrates by a simple hydro-thermal method. The morphology and structure of the products were characterized by scanning electron microscopy (SEM) and X-my dif-fraction analysis (XRD). A new method of substrate pretreatment was introduced to prepare ZnO coated films. The size of ZnO seeds and the formation rote of ZnO NTs were investigated. Further, the mechanism of the preparation of ZnO NTs was discussed. The photoluminescence (PL) spectrum measurement shows fairly internal defects existing in ZnO nanotubes.