ZrO2晶粒聚集态和粉末特性对增韧的影响

用 TEM 研究了热压 ZrO_2增韧 Al_2O_3(ZTA)的样品中,ZrO_2晶粒聚集态对四方相→单斜相相变的影响。以 Y_2O_3为稳定剂的四方 ZrO_2多晶体(Y-TZP)原料中加入同样组份的团聚粉末或粗粉末,对 ZrO_2的相变有很大影响。讨论了实验结果。对改善材料性能提出了建议。     

Y2O3添加对MA-CA2-CA6复合材料烧结行为的影响

为适应材料轻量化的发展需要,在1 400~1 600℃条件下制备了MA-CA_2-CA_6复合材料,并考察了添加Y_2O_3对该复合材料烧结行为的影响。结果表明,添加的Y_2O_3固溶入了CA_6、MA相中,Y~(3+)通过取代Ca~(2+)、Mg~(2+)有效地促进了MA晶粒的提前长大,抑制了CA_6晶粒的异常长大;另一方面,添加过量的Y_2O_3与体系中的Al_2O_3反应生成Y_3Al_5O_(12)新相,使得CA_6相的生成量减少,同时由于MA相提前长大限制了CA_6相的生长空间,进一步促进了CA_6晶粒形貌由片状向等轴状趋势发展。以上因素共同作用,促进了MA-CA_2-CA_6复合材料的烧结行为。当Y_2O_3的添加量为2%时,经1 600℃保温2h烧成后,试样的显气孔率由19.2%下降至4.8%,体积密度由2.78g/cm~3上升至3.24g/cm~3,制得的MA-CA_2-CA_6复合材料中MA、CA_2、CA_6及少量Y_3Al_5O_(12)晶相呈现交织分布,显微结构致密,力学性能得到改善。     

La2O3、Nd2O3、Y2O3对高岭石高温相变动力学的影响

利用综合热分析技术、X射线衍射(XRD)、傅里叶变换红外光谱(FT-IR)和扫描电镜(SEM)研究了La_2O_3、Nd_2O_3、Y_2O_3对高岭石高温条件下转变成莫来石过程的作用,并采用Kissinger方程、Ozawa方程以及JMA修正方程(Ⅰ)和(Ⅱ)分析了La_2O_3、Nd_2O_3、Y_2O_3对高岭石高温相变动力学的影响。结果表明:3种稀土氧化物的掺入对高岭石的相变动力学参数产生了影响,相变活化能和频率因子与未掺入稀土氧化物的高岭石相比有所降低,析晶方式则未发生变化,均属于体积晶化。对比掺入3种稀土氧化物的高岭石相变活化能和频率因子可以看出,Y_2O_3对于高岭石高温条件下相变的促进作用最为明显,相变活化能最低。稀土氧化物对于高岭石高温相变产物影响不大,主晶相为莫来石相,次晶相为方石英相,但稀土氧化物的掺入使得方石英相的结晶度明显提高。     

ZrO2—Al2O3陶瓷复合材料的研究与发展

自70年代发现在ZrO_2冲添加稳定剂能有效利用ZrO_2的马氏体相变来提高陶瓷材料的断裂韧度和强度以来,人们对ZrO_2陶瓷的增韧、增强及制备进行了大量而广泛的研究。迄今已有多种增韧氧化锆陶瓷进入实用阶段。但在Al_2O_3基质中分散ZrO_2粒子韧化氧化铝陶瓷的概念却是最近十来年才认识的。ZrO_2增韧Al_2O_3(简称ZTA)陶瓷复合材料作为第二代韧化陶瓷充分展示了它的潜力,现在其断裂韧度最高可达17MPam~(1/2),强度最高可达2400MPa,比通常陶瓷材料提高了3～5倍。     

Al2O3基陶瓷材料增韧的研究进展

Al_2O_3基陶瓷材料具有高的化学稳定性,有较好的应用前景,但其脆性限制了它的推广应用,对氧化铝陶瓷进行增韧是解决其脆性问题的一条重要途径。简要介绍了目前氧化铝陶瓷的增韧方法和增韧机理,综述了氧化铝陶瓷增韧的研究现状,分析了氧化铝陶瓷增韧研究中存在的主要问题,展望了氧化铝陶瓷增韧的发展方向,提出了原位生长及复合增韧是高性能Al_2O_3基陶瓷材料的研究重点。     

添加La2O3对粉煤灰合成Al2O3-SiC复合粉体的影响

以粉煤灰和活性炭为原料,通过碳热还原反应在Ar气氛下合成Al_2O_3-SiC粉体,探究了一条低成本合成Al_2O_3-SiC粉体的可行途径。研究了添加La_2O_3对合成过程的影响。采用XRD和SEM表征了材料的物相组成和显微形貌。结果表明:当粉煤灰与活性炭质量比为100∶44,在1 550℃下保温5h,添加6%(质量分数)的La_2O_3时,可合成性能良好的Al_2O_3-SiC粉体,颗粒分布均匀,平均粒径为0.5~1μm,较不添加La_2O_3合成温度降低约50℃。     

微波和真空烧结制备La2O3掺杂Al2O3透明陶瓷

通过共沉淀法制备La2O3掺杂Al_2O_3纳米粉,粉体经压制后分别采用微波和真空烧结制备Al_2O_3透明陶瓷。结果表明:Al_2O_3粉末颗粒大小均匀,近似球形,为40~60nm;两种烧结方式制备的试样XRD图中均为α-Al_2O_3,未检测到其它相。La2O3掺杂量为1%时,随烧结温度升高,两种烧结方法得到的Al_2O_3陶瓷的相对密度和抗弯强度均呈上升趋势,且微波烧结陶瓷的相对密度和抗弯强度明显高于真空烧结。1500℃烧结时,随La2O3掺杂量的增加,Al_2O_3陶瓷的相对密度均先增大后减小,当La2O3掺杂量为1%时,Al_2O_3陶瓷的相对密度和抗弯强度均最大。微波烧结陶瓷的透光率明显高于真空烧结,且其断口晶粒比真空烧结明显细少。     

粉末增塑挤压制备Al2O3/430L复合型蜂窝材料的组织与性能

为制备性能优良的Al_2O_3/430L复合型蜂窝载体材料,本文以430L不锈钢合金粉末、Al_2O_3粉末、粘结剂为原料,采用粉末增塑挤压技术挤压成形,并在1 100℃真空中烧结2 h获得Al_2O_3/430L复合型蜂窝材料.借助SEM、XRD及万能试验机,研究了添加Al_2O_3对Al_2O_3/430L复合型蜂窝材料的组织与性能的影响.研究表明:金属粉末颗粒在烧结过程中结合形成的基体组织为α-Fe(Cr),在基体晶粒间孔隙处和表面弥散分布着Al_2O_3颗粒.添加少量的Al_2O_3可提高烧结密度,制件表面光滑.随着Al_2O_3添加量增加,蜂窝材料表面负载催化涂层的能力增强;抗压强度随Al_2O_3添加量的增加先升高后降低,在Al_2O_3含量为2.5wt.%时,最大抗压强度达27 MPa.添加2.5wt.%Al_2O_3所制备的Al_2O_3/430L复合型蜂窝材料力学性能最佳、表面负载催化涂层的能力优良.     

Al2O3/B4C复相陶瓷制备及其韧化机理的研究进展

Al_2O_3/B_4C作为一种优良的结构部件,在工业及国防领域都具有广阔的应用前景。简要论述了Al_2O_3/B_4C复相陶瓷材料的几种常用制备方法,如自蔓燃高温合成、无压烧结法、热压烧结法、机械合金化法等;重点综述了Al_2O_3/B_4C复相陶瓷材料的几种增韧方式及增韧机理,并简述了Al_2O_3/B_4C复相陶瓷材料的应用;最后,指出了Al_2O_3/B_4C复相陶瓷材料的研究不足之处以及下一步的研究动向。     

La2O3对高钛高炉渣制备微晶泡沫玻璃的影响

利用高钛高炉水淬渣和废玻璃粉为基础原料,以CaCO_3为发泡剂,Na2B4O7·10H_2O为助熔剂,Na_3PO_4·12H_2O为稳泡剂,通过"一步法"烧结制备微晶泡沫玻璃,研究了La_2O_3的添加对微晶泡沫玻璃物相、结构及性能的影响。结果表明,添加La_2O_3对晶相种类改变不明显,但会提高晶化程度。随着La_2O_3添加量由0%(质量分数,下同)增至1.5%,微晶泡沫玻璃的气孔孔径减小,晶粒由粒状变为短棒状,微晶泡沫玻璃的体积密度、抗压强度升高,气孔率、吸水率和导热系数降低。La_2O_3添加量继续由1.5%增至3.5%,微晶泡沫玻璃的气孔孔径增大,晶粒尺寸逐渐变小直至呈现无规则形状,微晶泡沫玻璃的体积密度、抗压强度降低,气孔率、吸水率和导热系数升高。当La_2O_3添加量为1.5%时,所制得的微晶泡沫玻璃的综合性能最佳。     

Er3+/Yb3+掺杂NaGd(WO4)2粉体的制备与发光性能

采用水热法成功制备了Er~(3+)/Yb~(3+)双掺杂的NaGd(WO_4)_2纳米粉体,研究了不同络合剂、水热温度对样品形貌和结构的影响。测量了不同Er~(3+)掺杂浓度样品的可见上转换和近红外发射光谱。结果表明:在980nm LD激发下,可观测到样品强烈的绿色上转换发光,对应Er~(3+)的~2H_(11/2)→~4I_(15/2)(530nm)和~4S_(3/2)→~4I_(15/2)(552nm)跃迁,以及较弱的红色上转换和近红外发光,分别对应Er~(3+)的~4F_(9/2)→4I15/2(656nm)和~4I_(13/2)→~4I_(15/2)(1 532nm)跃迁。且随着Er~(3+)掺杂浓度的增加,样品的上转换红绿光和1.54μm附近的近红外光均呈现出先增大后减小的趋势。样品的激发和发射光谱显示,在378nm处的激发峰最强,对应Er~(3+)的~4I_(15/2)→~4 G_(11/2)能级跃迁,最强发射峰位于552nm。根据泵浦功率与发光强度的关系可以得出,红光和绿光的发射主要为双光子吸收过程,但红光还包含了一定的单光子吸收成分。     

Preparation and studies of Eu and Tb co-doped Gd2O3 and Y2O3 sol-gel scintillating films

Eu³⁺ (2.5 at.%) and Tb³⁺ (0.005-0.01 at.%) co-doped gadolinium and yttrium oxide (Gd₂O₃ and Y₂O₃) powders and films have been prepared using the sol-gel process. High density and optical quality thin films were prepared with the dip-coating technique. Gadolinium (III) 2,4-pentadionate and yttrium (III) 2,4-pentadionate were used as precursors, and europium and terbium in their nitrate forms were used as doping agents. Chemical and structural analyses (infrared spectroscopy, X-ray diffraction and high-resolution transmission electron microscopy) were conducted on both sol-gel precursor powders and dip-coated films. The morphology of thin films heat-treated at 700 °C was studied by means of atomic force microscopy. It was shown that the highly dense and very smooth films had a root mean roughness (RMS) of 2 nm ± 0.2 (A = 0.0075 Tb³⁺) and 24 nm ± 3.0 (B = 0.01 Tb³⁺). After treatment at 700 °C, the crystallized films were in the cubic phase and presented a polycrystalline structure made up of randomly oriented crystallites with grain sizes varying from 20 to 60 nm. The X-ray induced emission spectra of Eu³⁺- and Tb³⁺-doped Gd₂O₃ and Y₂O₃ powders showed that Tb³⁺ contents of 0.005, 0.0075 and 0.01 at.% affected their optical properties. Lower Tb³⁺ concentrations (down to 0.005 at.%) in both systems enhanced the light yield.     

Transparent Ga and Zn co-doped In2O3 electrode prepared by co-sputtering of Ga:In2O3 and Zn:In2O3 targets at room temperature

This study examined the characteristics of Ga:In₂O₃ (IGO) co-sputtered Zn:In₂O₃ (IZO) films prepared by dual target direct current (DC) magnetron sputtering at room temperature in a pure Ar atmosphere for transparent electrodes in IGZO-based TFTs. Electrical, optical, structural and surface properties of Ga and Zn co-doped In₂O₃ (IGZO) electrodes were investigated as a function of IGO and IZO target DC power during the co-sputtering process. Unlike semiconducting InGaZnO₄ films, which were widely used as a channel layer in the oxide TFTs, the co-sputtered IGZO films showed a high transmittance (91.84%) and low resistivity (4.1 × 10^− 4 Ω cm) at optimized DC power of the IGO and IZO targets, due to low atomic percent of Ga and Zn elements. Furthermore, the IGO co-sputtered IZO films showed a very smooth and featureless surface and an amorphous structure regardless of the IGO and IZO DC power due to the room temperature sputtering process. This indicates that co-sputtered IGZO films are a promising S/D electrode in the IGZO-based TFTs due to their low resistivity, high transmittance and same elements with channel InGaZnO₄ layer.     

Growth of La2Mo2O9 films on porous Al2O3 substrates by radio frequency magnetron sputtering

Synthesis conditions of La₂Mo₂O₉ thin film by radio frequency (RF) sputtering technique on Al₂O₃ ceramic substrates are studied. It is found that the deposition temperature and oxygen partial pressure are the most important factors for obtaining pure La₂Mo₂O₉ films. Varying both parameters, Mo-rich, stoichiometric, and Mo-deficient films are obtained. With increasing the La:Mo ratio, films become denser. A crust layer is observed on top of the Mo-rich and the Mo-deficient films. The formation of the La₂Mo₂O₉ phase is discussed with respect to the sputtering mechanism.     

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.     

Preparation and photoluminescence properties of Eu-doped Ga2O3 nanorods

GaOOH:Eu³⁺ nanorods with different aspect ratios were prepared by hydrothermal method at 140 °C. - and β-Ga₂O₃:Eu³⁺ were converted from as-prepared GaOOH:Eu³⁺ particles by calcination at 500 and 850 °C, respectively. The products were characterized with X-ray diffraction (XRD), transmission electron microscope (TEM) and photoluminescence (PL). Results show that solution pH values play a key role in the formation of the GaOOH:Eu³⁺ powders with different morphologies and - and β-Ga₂:Eu³⁺ inherit the morphology of GaOOH:Eu³⁺ exactly. The photoluminescence characteristics of β-Ga₂O₃:Eu³⁺ were also investigated. Experimental results reveal that the color purity of β-Ga₂O₃:Eu³⁺ nanorods with high aspect ratio is enhanced in comparison with β-Ga₂O₃:Eu³⁺ nanorods with low aspect ratio.     

Varistor properties of ZnO-Pr6O11-CoO-Cr2O3-Y2O3-In2O3 ceramics

The varistor properties of the ZnO-Pr₆O₁₁-CoO-Cr₂O₃-Y₂O₃-In₂O₃ ceramics were investigated for different concentrations of In₂O₃. The increase of In₂O₃ concentration slightly increased the sintered density (5.60-5.63 g/cm³) and slightly decreased the average grain size (3.4-2.9 μm). The breakdown field increased from 6023 to 14822 V/cm with increasing concentration of In₂O₃. The nonlinear coefficient increased from 17.6 to 44.6 for up to 0.005 mol%, whereas the further doping caused it to decrease to 36.8. In₂O₃ acted as an acceptor due to the donor concentration, which decreases in the range of 1.02 × 10¹⁷ to 0.24 × 10¹⁷/cm³ with increasing concentration of In₂O₃.     

Fabrication of Y2O3-doped BaZrO3 thin films by electrostatic spray deposition

Electrostatic spray deposition (ESD) technique was used to fabricate dense Y₂O₃-doped BaZrO₃ (BYZ) thin films, which have been extensively studied for the protonic ceramic fuel cell electrolyte. Effects of the ESD process parameters (i.e. substrate temperature, type of precursor, flow rate and applied voltage) on the microstructure of as-deposited films were studied. The uniform as-deposited films were obtained using a mixture of zirconium acetylacetonate, barium chloride dihydrate and yttrium chloride hexahydrate precursors in a solvent mixture of butyl carbitol and deionized water at a volume ratio of 50:50. The optimum deposition parameters were obtained at the substrate temperature of 250 °C with the applied voltage and flow rate in a range of 10-12 kV and 1.4-2.8 ml/h, respectively. The as-deposited films were subsequently annealed at 1350 °C for 10 h to ensure the complete chemical reactions of the precursors. X-ray diffraction patterns reveal the perovskite structures of the annealed BYZ films (deposited on yttria stabilized zirconia substrates) with only traces of Y₂O₃ phase, which could arise from the loss of BaO at high annealing temperatures.     

Stability and effect of annealing on the optical properties of plasma-deposited Ta2O5 and Nb2O5 films

Tantalum and niobium oxide optical thin films were prepared at room temperature by plasma-enhanced chemical vapor deposition using tantalum and niobium pentaethoxide (M(OC₂H₅)₅) precursors. We studied the evolution of their optical and microstructural properties as a result of annealing over a broad temperature range from room temperature up to 900 °C. The as-deposited films were amorphous; their refractive index, n, and extinction coefficient, k, at 550 nm were n = 2.13 and k < 10^− 4 for Ta₂O₅, and n = 2.24 and k < 10^− 4 for Nb₂O₅. The films contained a small amount of residual carbon (∼ 2-6 at.%) bonded mostly to oxygen. During annealing, the onset of crystallization was observed at approximately T_C1 = 650 °C for Ta₂O₅ and at T_C1 = 450 °C for Nb₂O₅. Upon annealing close to T₁ (300 °C for Nb₂O₅ and 400 °C for Ta₂O₅), n at 550 nm decreased by less than 1%. This was correlated with the decrease of carbon content, as suggested by Fourier transform infrared spectroscopy, elastic recoil detection and static secondary ion mass spectroscopy (SIMS) results. During annealing, we observed phase transition from the δ- (hexagonal) phase to the L- (orthorhombic) phase between 800 °C and 900 °C for Ta₂O₅, and between 600 °C and 700 °C for Nb₂O₅. The structural changes were also marked by silicon diffusion from the substrate into the oxide layer at annealing temperatures above 500 °C for Ta₂O₅ and above 400 °C for Nb₂O₅. As a consequence of oxygen, silicon and metal interdiffusion, the interface between the Si substrate and the metal oxide (Ta₂O₅ or Nb₂O₅) is characterized by its broadening, well documented by spectroscopic ellipsometry and SIMS data.