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 density of the target were inves- tigated. Also, a discussion was made on the sintering atmosphere.

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~C calcined particles had a crystallite size of 25.3 nm and a specific surface area of 26.1 m2.g i The avoidance of chlorine ions in the synthesis process decreases particle agglomeration and promotes powder densification. The 900~C sintered pellet had a density of 67.6% of theoretical density （TD） and increased steadily to 97.3% for the 1400℃ sintered ceramics, respectively.

Phase evolutions of two kinds of co-precipitated indium-tin oxide pre-cursors by heat-treatment

Two kinds of indium-tin oxide (ITO) precursors, cubic indium hydroxide(In(OH)_3) and orthorhombic indium oxide hydroxide (InOOH), were prepared by a co-precipitationmethod. With the help of X-ray diffraction (XRD), thermo-gravimetric analysis (TGA) and differentialthermal analysis (DTA), phase evolutions from cubic In(OH)_3 and orthorhombic InOOH to cubic ITOsolid solution and rhombohedral ITO solid solution by heat-treatment had been comprehensivelyinvestigated. The transformation from cubic In(OH)_3 to cubic ITO solid solution started as low as150 deg C and ended at about 300 degC, and it exhibited an endothermic behavior. The transformationfrom orthorhombic InOOH to rhombohedral ITO solid solution started at 220 deg C and ended at about430 deg C. Moreover, this transformation was composed of two processes: the one was the dehydrationof InOOH exhibiting an endothermic behavior and the other was the transformation from dehydrationproducts to rhombohedral ITO solid solution exhibiting a strong exothermic behavior. RhombohedralITO solid solution was metastable in air and it would transform to cubic ITO solid solution byheat-treatment. The transformation from rhombohedral ITO solid solution to cubic ITO solid solutionstarted at 578 deg C and ended below 800 deg C, and it exhibited a weak exothermic behavior.

Fabrication and Characterization of Glass-Ceramics Doped with Rare Earth Oxide and Heavy Metal Oxide

Cordierite-based glass-ceramics with non-stoichiometric composition doped with rare earth oxide (REO_2) and heavy metal oxide (M_2O_3) respectively were fabricated from glass powders. After sintering and crystallization heat treatment, various physical properties, including compact density and apparent porosity, were examined to evaluate the sintering behavior of cordierite-based glass-ceramics. Results show that the additives both heavy metal oxide and rare earth oxide promote the sintering and lower the phase temperature from μ- to α-cordierite as well as affect the dielectric properties of sintered glass-ceramics. The complete-densification temperature for samples is as low as 900 ℃. The materials have a low dielectric constant (≈5), a low thermal expansion coefficient ((2.80～3.52)×10^(-6) ℃^(-1)) and a low dissipation factor (≤0.2%) and can be co-fired with high conductivity metals such as Au, Cu, Ag/Pd paste at low temperature (below 950 ℃), which makes it to be a promising material for low-temperature co-fired ceramic substrates.

模压成型压力对氧化铟锡(ITO)靶材性能影响研究

以化学共沉淀-煅烧法制备的纳米ITO粉体为原料,通过模压、冷等静压成型,采用常压烧结法制备了ITO靶材,研究了模压成型压力对ITO靶材相对密度、电阻率和晶粒尺寸的影响。结果表明,模压成型压力60 MPa且烧结条件适宜时,制得的ITO靶材相对密度为99.81%、电阻率为1.707×10^(-4)Ω·cm、平均晶粒尺寸为7.62μm。研究结果可为ITO靶材的致密化与大型化生产提供借鉴。

A sol-gel method to synthesize indium tin oxide nanoparticles

Transparent conductive indium tin oxide （ITO） nanoparticles were synthesized by a novel sol-gel method. Granulated indium and tin were dissolved in HNO3 and partially complexed with citric acid. A sol-gel process was induced when tertiary butyl alcohol was added dropwise to the above solution. ITO nanopartides with an average crystallite size of 18.5 nm and surface area of 32.6 m^2 ]g were obtained after the gel was heat-treated at 700 ℃, The ITO nanoparticles showed good sinterability, the starting sintering temperature decreased sharply to 900 ℃, and the 1400 ℃ sintered pellet had a density of 98.1% of theoretical density （TD）.

高纯溅射靶材回收研究现状

高纯溅射靶材在晶圆代工企业和液晶面板企业作为耗材使用。高纯溅射靶材利用率低,一般平面靶利用率低于30%,旋转靶难超过70%,回收溅射后的残靶具有非常高的经济价值和环保意义。本文综述了贵金属、ITO、钛、钽、铝、铜等高纯靶材的回收研究现状,总结了靶材回收过程中面临的共同问题。目前在高纯靶材的残靶回收中还存在金属回收率低、回收的纯度不高、工艺流程长等问题需要攻克和改善,作者展望了开发较短的流程、环境友好的工艺、探索高价值的用途,是未来高纯残靶回收技术改进和发展的方向。

Synthesis of 3D ordered macroporous indium tin oxide using polymer colloidal crystal template

Three-dimensional (3D) ordered macroporous indium tin oxide (ITO) is pre- pared using a polymer colloidal crystal template that is formed by self-assembly of the monodisperse poly(methyl methacrylate) (PMMA) microspheres. The morphologies and BET surface area of the macroporous material is examined by scanning electron micro- scope, transmission electron microscopy and N2 adsorption/desorption. Results indicate that the macroporous material has highly ordered arrays of the uniform pores replicated from the PMMA colloidal crystal template when the polymer colloidal crystal template is removed by calcinations at 500℃. The pore diameter (about 450 nm) of macroporous ITO slightly shrank to the PMMA microspheres. The BET surface area and pore volume of the macroporous material are 389 m2·g-1 and 0.36 cm3·g-1, respectively. Moreover, the macroporous ITO, containing 5 mol% Sn and after annealing under vacuum, shows the minimum resistivity of ρ = 8.2×10-3 Ω· cm. The conductive mechanism of macroporous ITO is discussed, and it is believed that the oxygen vacancies are the major factor for excellent electrical properties.

Nb和TiB_(2)对ZrB_(2)基复合陶瓷材料组织及性能的影响

利用气压辅助烧结法制备ZrB_(2)基复合陶瓷材料,借助力学性能测试、XRD、SEM等探究了添加Nb与TiB_(2)对所制材料烧结行为、力学性能及抗氧化能力的影响。结果表明,金属Nb在烧结过程中发生塑性形变促使ZrB_(2)颗粒重排,同时破坏B—B共价键促进物质扩散,改善了材料的烧结及力学性能,但也造成材料高温抗氧化性能下降。进一步引入TiB_(2)能提高陶瓷材料的力学性能,且反应生成的ZrTiO4有利于形成抗氧化保护层以提高材料的高温抗氧化能力。

基于ITO柔性透明偏振不敏感超宽带超材料吸波器

设计了一种基于电阻膜氧化铟锡(ITO)的柔性透明偏振不敏感超宽带吸波器,并对其进行了分析和制备。利用ITO电阻膜图样产生欧姆损耗实现高吸收。仿真结果表明设计的超材料吸波器在2.7~12.1 GHz范围内可实现高于90%吸收率,相对带宽为127%,覆盖了S、C、X波段。由于结构的对称性,该吸波器对偏振角不敏感,且在45°宽入射角范围内具有高吸收率。通过阻抗匹配、等效电路理论、电场以及电流分布、结构参数分析了吸收机理。实验测量结果与仿真结果一致。该超材料吸波器具有超宽带吸收、极化不敏感和灵活性好等优点,可广泛应用于电磁屏蔽、雷达隐身技术等领域。

基底温度对射频磁控溅射PI基ITO薄膜的影响

采用射频(RF)磁控溅射法在柔性耐高温聚酰亚胺(PI)薄膜上沉积了氧化铟锡(ITO)薄膜,研究了基底温度对ITO薄膜性能的影响。运用四探针测试仪研究了基底温度对ITO薄膜方块电阻及电阻率的影响,并用扫描电子显微镜(SEM)、X射线衍射仪(XRD)研究了基底温度对ITO薄膜表面形貌及结晶度的影响。采用X射线光电子能谱仪(XPS)、附着力测试仪分析电学性能最优的样品化学组成与附着力。研究结果表明,ITO薄膜方块电阻及电阻率随基底温度上升先下降后上升,在基底温度为250℃时,ITO薄膜方块电阻为14.1Ω/□,电阻率为1.9×10^(-4)Ω·cm,基膜附着力好,薄膜结晶度高,(222)晶面存在择优取向。

优化基于PVP的有机双稳态存储器的电性能

在未来非易失性存储器的应用中,有机双稳态存储器具有良好的发展潜力,但仍缺少对提升存储器性能的简单方法的探究。制备了一系列基于聚(4-乙烯基苯酚)(PVP)的三明治结构的柔性存储器,发现结构为氧化铟锡(ITO)/聚(3-己基噻吩)(P3HT)(二氯苯(DCB))/PVP/Cu的存储器写入电压最低。使用全溶液方法在柔性基底上制备此结构的存储器,并测试了其电性能。结果表明,写入电压为1.0 V,开关(ON/OFF)比为1×10^(5),保留时间达到2×10^(4)s。同时,通过分析其开关机理解释了结构和材料影响存储器性能的原理,加入修饰层P3HT和将金属电极由Al改为Cu,均可使介电层和电极之间的能级更匹配,从而降低载流子运输需克服的势垒;使用X射线衍射仪(XRD)和紫外-可见(UV-Vis)光谱仪验证了将P3HT的溶剂氯苯换为二氯苯,可增强P3HT分子的有序形态和结晶度,从而提高电荷传输能力以降低存储器写入电压。这将从设计材料和优化结构方面为提高有机存储器性能提供参考。

二硼化锆陶瓷材料的研究及展望

随着高温技术的快速发展,高温材料的需求日益增大,同时对高温材料的性能提出了更高的要求。重点综述了高温材料中ZrB2陶瓷材料的原料、应用、烧结致密化技术、研究现状以及该种材料的氧化研究现状。从分析可以看出,其应用主要面临的问题是高温下易氧化、强度低、致密体的获得比较困难、成本较高及在热学和电学性能方面的研究较少。在研究ZrB2陶瓷的过程中,如能充分发挥其优点、改善其缺点和挖掘出更多的特性,必将使ZrB2陶瓷得到更大的发展。

HIT太阳电池中ITO薄膜的结构和光电性能

采用射频磁控溅射技术在不同射频功率下沉积了ITO薄膜,并将其应用于HIT太阳电池.分析了薄膜的结构、光电特性.结果表明,在120W时制备的薄膜很好地兼顾了电阻率和光透过率,其电阻率为3.48×10^-4Ω·cm、在350～800 nm波段的平均光透过率为87.1%,将其应用于HIT太阳电池上,电池的转换效率可达13.38%.

硝酸氧化法氧化锡陶瓷材料的制备、掺杂与气敏性能

采用正交试验法研究了硝酸氧化法ＳｎＯ２陶瓷材料的工艺条件对ＳｎＯ２收率和环境的影响。用Ｘ射线衍射法测得了不同热处理温度下陶瓷材料的晶体结构，并计算了平均晶粒尺寸。研究了晶粒尺寸和贵金属掺杂对ＳｎＯ２气敏性能的影响，得到了ＳｎＯ２气敏陶瓷的优化工艺条件。

α-Sialon柱状晶的制备

研究了α－Ｓｉａｌｏｎ柱状晶制备过程．结果表明，α－Ｓｉａｌｏｎ柱状晶可以通过无压烧结和酸洗的方法制备得到．α－Ｓｉａｌｏｎ柱状晶形貌与添加剂种类有关，选用轻稀土氧化物为添加剂制得的α－Ｓｉａｌｏｎ柱状晶具有较小的直径和较大的长径比，而选用重稀土氧化物为添加剂的α－Ｓｉａｌｏｎ柱状晶的直径较大，长径比较小．文中就添加剂种类对α－Ｓｉａｌｏｎ柱状晶形貌的影响进行了讨论．

溶剂热-煅烧法合成纳米ITO粉体

本文采用溶剂热-煅烧法制备纳米铟锡复合氧化物(ITO)。以In(4N)、SnCl4.5H2O为起始原料,通过XRD、SEM及微波吸收性能的分析,考察了溶剂热反应中溶剂对ITO粉体结构及性能的影响。研究表明以1,4-丁二醇为溶剂,KBr为矿化剂(浓度0.5mol/L)在260℃下醇热6h,得到结晶性良好的羟基氧化铟和锡掺杂氧化铟的混合物。溶剂热产物在550℃下煅烧2h得到纳米ITO粉体,醇热-煅烧产物的吸波性能良好。

低发射率涂层材料研究

测试了多种黏合剂和粉体及以聚氨酯树脂为黏合剂制成的涂膜在8～14μm波段的发射率。结果表明，Karton树脂红外透明性好，具有较低的红外发射率；铝粉制成涂膜后发射率较低，且涂膜的发射率与铝粉的加入量、粒径等有关；掺锡氧化铟（ITO）薄膜具有很低的发射率，其发射率与ITO膜的厚度、含氧量等有关。

掺杂ZnSnO_3气敏特性及实用性研究

本文通过对ZnSnO3传感器进行各种掺杂来提高其灵敏度、选择性和工作温度。结果发现 :在所有的掺杂剂中 ,TiO2 能显著提高其灵敏度而且灵敏度是无掺杂ZnSnO3传感器的两倍多 ,并且最佳的掺杂量为 5 %mol。此外 ,这种掺杂ZnSnO3传感器的回复 响应时间为 10S左右 ,足够实际应用。在有其它气体存在的情况下 ,这种掺杂ZnSnO3传感器仍然对乙醇具有较高的选择性。用SEM对其进行了解释。因此 ,掺TiO2 的ZnSnO3传感器对乙醇具有较高的灵敏度并且保持较高的选择性 ,能够重复使用以及 6 0h后 ,其灵敏度可保持稳定值。

掺Yb^(3+)氧化镧钇透明激光陶瓷的光谱特性

采用传统陶瓷烧结工艺,在无压还原气氛下低温制备出透明性良好的掺Yb3+氧化镧钇透明激光陶瓷,测试了其在室温下的吸收光谱、发射光谱和荧光寿命.结果表明,掺Yb3+氧化镧钇透明激光陶瓷的吸收系数随着Yb3+掺杂浓度的增加而增大,最强吸收峰974 nm处的吸收截面为0.90~1.12×10-20cm2;主发射峰1 032 nm和1 075 nm处的发射截面分别为1.05×10-20cm2和0.87×10-20cm2;Yb3+掺杂浓度为5at.%时荧光寿命为1.38 ms,并随Yb3+掺杂浓度的增加而减小;当Yb3+掺杂浓度超过10at.%时,样品中存在严重的浓度猝灭.产生浓度猝灭的原因是高掺杂时离子间存在合作上转换和能量转移.