Synthesis and characterization of Al2O3 hollow spheres

This paper presents a novel technique to create Al₂O₃ hollow spherical nanoparticles. It used Al(OH)₃ which was synthesized with Al₂(SO₄)₃ and NaOH, and the C-Al(OH)₃ core-shell nanoparticle as intermediate phases. The Al₂O₃ hollow spheres were achieved by the calcination of the carbon cores and the dehydration of Al(OH)₃. The chemical composition, morphology, size and superficial crystal structure of the nanoparticles were characterized with TEM, XRD, TGA, FTIR and BET. The result shows that the average diameter of the C-Al(OH)₃ core-shell nanoparticles is about 25 nm, the thickness of the Al₂O₃ shell is about 5 nm and the surface area is 215.2 m²/g. The procedure for the formation of Al₂O₃ hollow nanoparticles is discussed in details.     

The etching characteristics of Al2O3 thin films in an inductively coupled plasma

In this study, the etching characteristics of ALD deposited Al₂O₃ thin film in a BCl₃/N₂ plasma were investigated. The experiments were performed by comparing the etch rates and the selectivity of Al₂O₃ over SiO₂ as functions of the input plasma parameters, such as the gas mixing ratio, the DC-bias voltage, the RF power, and the process pressure. The maximum etch rate was obtained at 155.8 nm/min under a 15 mTorr process pressure, 700 W of RF power, and a BCl₃ (6 sccm)/N₂ (14 sccm) plasma. The highest etch selectivity was 1.9. We used X-ray photoelectron spectroscopy (XPS) to investigate the chemical reactions on the etched surface. Auger electron spectroscopy (AES) was used for the elemental analysis of the etched surfaces.     

Thermo-optic properties of TiO2, Ta2O5 and Al2O3 thin films for integrated optics on silicon

The direct measurement of the thermo-optic coefficients of aluminium oxide, tantalum pentoxide and titanium dioxide thin films is presented. Using ellipsometry on monolithically integrated permutations of the layers of silicon, silicon dioxide and the material under test, allows the direct measurement of the overall thermo-optic coefficient accounting for thermally induced changes in the dielectric permittivity and density of the materials as well as the elasto-optic effect due to the non-matching thermal expansion coefficients of the different materials.     

Etching characteristics of Al2O3 thin films in inductively coupled BCl3/Ar plasma

The investigation of Al₂O₃ etch characteristics in the BCl₃/Ar inductively coupled plasma was carried out in terms of effects of input process parameters (gas pressure, input power, bias power) on etch rate and etch selectivity over poly-Si and photoresist. It was found that, with the changes in gas pressure and input power, the Al₂O₃ etch rate follows the behavior of ion current density while the process rate is noticeably contributed by the chemical etch pathway. The influence of input power on the etch threshold may be connected with the concurrence of chemical and physical etch pathways in ion-assisted chemical reaction.     

Microstructure and electrical properties of Al2O3-ZrO2 composite films for gate dielectric applications

Al₂O₃-ZrO₂ composite films were fabricated on Si by ultrahigh vacuum electron-beam coevaporation. The crystallization temperature, surface morphology, structural characteristics and electrical properties of the annealed films are investigated. Our results indicate that the amorphous and mixed structure is maintained up to an annealing temperature of 900 °C, which is much higher than that of pure ZrO₂ film, and the interfacial oxide layer thickness does not increase after annealing at 900 °C. However, a portion of the Al₂O₃-ZrO₂ film becomes polycrystalline after 1000 °C annealing and interfacial broadening is observed. Possible explanations are given to explain our observations. A dielectric constant of 20.1 is calculated from the 900 °C-annealed ZrO₂-Al₂O₃ film based on high-frequency capacitance-voltage measurements. This dielectric characteristic shows an equivalent oxide thickness (EOT) as low as 1.94 nm. An extremely low leakage current density of ∼2×10⁻⁷ A/cm² at a gate voltage of 1 V and low interface state density are also observed in the dielectric film.     

Tensile strength and microstructure of Al2O3-ZrO2 hypo-eutectic fibers

Al₂O₃-ZrO₂(Y₂O₃) eutectic materials possess good fracture strengths and creep resistance. Increased Al₂O₃ content is one means to further improve creep resistance. The objective of this study is to examine fracture strength of Al₂O₃-rich (hypoeutectic) compositions at varying Y₂O₃ contents. Fibers 160-220 μm in diameter with 68 m/o Al₂O₃ and 1.1-7.6 m/o Y₂O₃ (30.5 to 16 m/o ZrO₂) were directionally solidified at 0.11 mm/s using the laser-heated float-zone process. Defect populations increased in size and severity with higher Y₂O₃ contents. However, fibers maintained 1 GPa fracture strength in the presence of numerous pores and shrinkage cavities, which extend with crack-like morphology along the fiber axis.     

Properties of polyimide/Al2O3 and Si3N4 deposited thin films

Polyimide (PI) nanocomposites with different proportions of Al₂O₃ were prepared via two-step reaction. Silicon nitride (Si₃N₄) was deposited on PI composite films by a RF magnetron sputtering system and used as a gas barrier to investigate the water vapor transmission rate (WVTR). The thermal stability and mechanical properties of a pure PI film can be improved obviously by adding adequate content of Al₂O₃. At lower sputtering pressure (4 mTorr), the PI/Al₂O₃ hybrid film deposited with Si₃N₄ barrier film exhibits denser structure and lower root mean square (RMS) surface roughness (0.494 nm) as well as performs better in preventing the transmission of water vapor. The lowest WVTR value was obtained from the sample, 4 wt.%Al₂O₃-PI hybrid film deposited with Si₃N₄ barrier film with the thickness of 100 nm, before and after bending test. The interface bonding, Al-N and Al-O-Si, was confirmed with the XPS composition-depth profile.     

Synthesis of GaN nanorods by ammoniating Ga2O3 films on In2O3 layer deposited on Si (111) substrates

GaN nanorods were synthesized by ammoniating Ga₂O₃/In₂O₃ thin films deposited on Si (111) with magnetron sputtering. X-ray diffraction, Scanning electronic microscope and high-resolution TEM results show that they are GaN single crystals, the sizes of which vary from 2 to 7 μm in length and 200 to 300 nm in diameter. In₂O₃ middle layer plays an important role in the GaN nanorod growth.     

Y2O3添加量对Al2O3/ZrO2共晶陶瓷显微组织及力学性能的影响

为探索第三组元Y₂O₃添加对Al₂O₃/ZrO₂共晶陶瓷显微组织与机械性能的影响,本文利用低温度梯度的高温熔凝法制备了直径为20 mm的Al₂O₃/ZrO₂(Y₂O₃)共晶陶瓷块体,采用SEM、EDS及XRD技术对共晶陶瓷进行微结构分析,并利用维氏压痕法对其硬度和断裂韧性进行测试。SEM结果表明,凝固组织由群集的共晶团结构组成,随着Y₂O₃添加量的增加,共晶团形态由胞状转变为枝晶状,内部相间距在1~2 μm范围内变化。力学测试表明,Y₂O₃摩尔分数小于1.1%时,由于组织内部存在低硬度m-ZrO₂及微裂纹缺陷,故陶瓷硬度较低,约为(9.53±0.22 )GPa;当Y₂O₃摩尔分数为1.1%时,陶瓷硬度最大,约为(18.05±0.27)GPa;当Y₂O₃的摩尔分数大于1.1%时,由于共晶团边界区内气孔缺陷及粗大组织增多,引起陶瓷硬度值略有下降。低Y₂O₃摩尔分数添加时,陶瓷断裂韧性相对较高,约为(6.30±0.16)MPa·m^1/2,这与其内部存在大量微裂纹缺陷有关;随着Y₂O₃添加量的增加,陶瓷的微裂纹数量减少、边界区内缺陷增多,断裂韧性降低。     

Mechanical properties and microstructure of Al2O3/TiAl in situ composites doped with Cr2O3

Al₂O₃/TiAl composites were successfully fabricated from powder mixtures of Ti, Al, TiO₂ and Cr₂O₃ by a hot-press-assisted exothermic dispersion method. The effect of the Cr₂O₃ addition on the microstructures and mechanical properties of Al₂O₃/TiAl composites was characterized, and the results showed that the Rockwell hardness, flexural strength and fracture toughness of the composites increased as the Cr₂O₃ content increased. When the Cr₂O₃ content was 2.5 wt%, the flexural strength and the fracture toughness attained peak values of 925 MPa and 8.55 MPa m^1/2, respectively. This improvement of mechanical properties was due to the more homogeneous and finer microstructure developed from the addition of Cr₂O₃ and an increase in the ratio of α₂-Ti₃Al to γ-TiAl matrix phases.     

Combined spectroscopic ellipsometry and attenuated total reflection analyses of Al2O3/HfO2 nanolaminates

The microstructure of thin HfO₂-Al₂O₃ nanolaminate high κ dielectric stacks grown by atomic vapor deposition has been studied by attenuated total reflection spectroscopy (ATR) and 8 eV spectroscopic ellipsometry (SE). The presence of Al₂O₃ below HfO₂ prevents the crystallisation of HfO₂ if an appropriate thickness is used, which depends on the HfO₂ thickness. A thicker Al₂O₃ is required for thicker HfO₂ layers. If crystallisation does occur, we show that the HfO₂ signature in both ATR and 8 eV SE spectra allows the detection of monoclinic crystallites embedded in an amorphous phase.     

Lightweight geopolymer made of highly porous siliceous materials with various Na2O/Al2O3 and SiO2/Al2O3 ratios

The syntheses of lightweight geopolymeric materials from highly porous siliceous materials viz. diatomaceous earth (DE) and rice husk ash (RHA) with high starting SiO₂/Al₂O₃ ratios of 13.0-33.5 and Na₂O/Al₂O₃ ratios of 0.66-3.0 were studied. The effects of fineness and calcination temperature of DE, concentrations of NaOH and KOH, DE to RHA ratio; curing temperature and time on the mechanical properties and microstructures of the geopolymer pastes were investigated. The results indicated that the optimum calcination temperature of DE was 800 °C. Increasing fineness of DE and starting Na₂O/Al₂O₃ ratio resulted in an increase in compressive strength of geopolymer paste. Geopolymer pastes activated with NaOH gave higher compressive strengths than those with KOH. The optimum curing temperature and time were 75 °C and 5 days. The lightweight geopolymer material with mean bulk density of 0.88 g/cm³ and compressive strength of 15 kg/cm² was obtained. Incorporation of 40% RHA to increase starting SiO₂/Al₂O₃ and Na₂O/Al₂O₃ ratios to 22.5 and 1.7 and enhanced the compressive strength of geopolymer paste to 24 kg/cm² with only a marginal increase of bulk density to 1.01 g/cm³. However, the geopolymer materials with high Na₂O/Al₂O₃ (>1.5) were not stable in water submersion.     

Electrical characteristics of Ti-O/Ta2O5 thin film sputtered on Ta/Ti/Al2O3 substrate

The electrical characteristics of Ti-O/Ta₂O₅ films sputtered on Ta/Ti/Al₂O₃ substrate were investigated. Ta (tantalum) was used for the bottom and upper electrodes for the purpose of simplifying the fabrication process and Al₂O₃ substrates were used, which are needed in integral passive devices. Ta/Ti-O/Ta₂O₅/Ta/Ti/Al₂O₃ capacitors were annealed at 700 °C for 60 s in vacuum. The X-ray diffraction pattern (XRD) results showed that as-deposited Ta had a highly preferred orientation, but Ta₂O₅ film had amorphous structure, which was transformed to crystallization structure by rapid thermal heat treatment. We examined the log J-E and C-V characteristics of the dielectric thin films deposited on the Ta bottom electrode. From these results, we concluded that the leakage current could be reduced by introducing a Ti-O buffer layer. The conduction mechanisms of Ta/Ti-O/Ta₂O₅/Ta/Ti/Al₂O₃ capacitors could be interpreted appropriately by hopping conduction in lower field (E<1×10⁵ V/cm) and space-charge-limited current in higher fields (1×10⁵ V/cm<E).     

Structure and property changes of ZrO2/Al2O3/ZrO2 laminate induced by low-temperature NH3 annealing applicable to metal-insulator-metal capacitor

Phase transformation and morphology evolution of ZrO₂/Al₂O₃/ZrO₂ laminate induced by the post-deposition NH₃ annealing at 480 °C were studied and the effect on the electrical property of the TiN/ZrO₂/Al₂O₃/ZrO₂/TiN capacitor module was evaluated in dynamic random access memory cell. Experimental results indicated N could indeed be incorporated into the dielectric laminate by the low-temperature NH₃ annealing, resulting in tetragonal-to-cubic phase transformation and small crystallites in the ZrO₂ layers. The C residue and Cl impurity in the ZrO₂/Al₂O₃/ZrO₂ laminate, which derived from the dielectric film formation and capping TiN layer deposition, respectively, could also be reduced by the nitridation process. As a result of the better surface morphology and less impurity content, lower dielectric leakage current and longer reliability lifetime were observed for the nitrided ZrO₂/Al₂O₃/ZrO₂ capacitor. This study demonstrates the low-temperature NH₃ annealing on ZrO₂/Al₂O₃/ZrO₂ dielectric can be applicable to the metal-insulator-metal capacitor structure with nitride-based electrode, which brings advantages over mass production-wise property improvements and extends the practical applicability of the ZrO₂/Al₂O₃/ZrO₂ dielectric.     

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℃。     

MgO/Al2O3比对MgO-Al2O3-SiO2系统玻璃分相与析晶的影响

采用高温熔融法制备了具有不同MgO/Al₂O₃比的堇青石微晶玻璃。采用差热分析仪(DTA)、X射线衍射仪(XRD)、扫描电子显微镜(SEM)等测试技术研究了MgO/Al₂O₃比对该系统玻璃分相和析晶的影响。结果表明:当SiO₂含量不变时,随着MgO/Al₂O₃比的减小,分相形貌由连通的蠕虫状逐渐变为孤立的球形结构,且分相粒子尺寸逐渐减小,从200~300 nm减小至30~50 nm。当MgO/Al₂O₃比从3降到1,析晶峰温度由997 ℃升至1 105 ℃,析晶的难度逐渐提高。当MgO/Al₂O₃比为3时,MgO-Al₂O₃-SiO₂系统玻璃经950 ℃热处理后即产生大量分相,经1 050 ℃热处理后在分相液滴中析出大量堇青石晶体,且堇青石优先在富Mg相中析出。提高MgO/Al₂O₃比有利于MgO-Al₂O₃-SiO₂系统玻璃在分相中析晶,反之,则会降低系统的分相和析晶能力。     

Al2O3/Al-4.5Cu-Ce合金复合材料的界面现象

本研究采用座滴法和电子探针探讨了Al-4.5Cu-Ce合金的表面张力及其与Al₂O₃的界面润湿性、界面结构、界面结合方式和强度.得出:饰降低Al-4.5Cu合金的表面张力,提高Al₂O₃/Al-4.5Cu合金的润湿性和界面剪断应力;铈改善润湿性的机制是在界面上的吸附与富集,未发现铈与Al₂O₃的界面反应产物,界面仍属于直接结合界面.     

Al2O3短纤维/Al-12Si复合材料启裂特征的TEM原位观察研究

利用挤压铸造法制备了Al₂O₃(15%)/Al-12Si复合材料,并采用透射电镜动态拉伸技术对复合材料的裂纹形成及微观断裂过程进行了原位观察,发现该复合材料的纤维/基体界面是破坏路径之一,并发现了纤维中裂纹形成及扩展至完全破坏的现象.     

Structural and electrical properties of HfO2/Dy2O3 gate stacks on Ge substrates

In the present work we report on the structural and electrical properties of metal-oxide-semiconductor (MOS) devices with HfO₂/Dy₂O₃ gate stack dielectrics, deposited by molecular beam deposition on p-type germanium (Ge) substrates. Structural characterization by means of high-resolution Transmission Electron Microscopy (TEM) and X-ray diffraction measurements demonstrate the nanocrystalline nature of the films. Moreover, the interpretation of the X-ray reflectivity measurements reveals the spontaneous growth of an ultrathin germanium oxide interfacial layer which was also confirmed by TEM. Subsequent electrical characterization measurements on Pt/HfO₂/Dy₂O₃/p-Ge MOS diodes show that a combination of a thin Dy₂O₃ buffer layer with a thicker HfO₂ on top can give very good results, such as equivalent oxide thickness values as low as 1.9 nm, low density of interfacial defects (2-5 × 10¹² eV^− 1 cm^− 2) and leakage currents with typical current density values around 15 nA/cm² at V_g = V_FB − 1V.     

Enhanced ferroelectric properties of Fe-doped BaTiO3 thin film deposited on LaNiO3/Si substrate by sol–gel technique

The ferroelectric thin films of Fe-doped BaTiO₃ and undoped BaTiO₃ were prepared on LaNiO₃ coating Si substrates by sol–gel technique. It was found that a small amount of Fe dopant could significantly enhance the ferroelectric properties of the BaTiO₃ thin film. The remnant polarization of Fe-doped BaTiO₃ thin film at room temperature reached to 14.9 μC/cm². The loss tangent, compared to the undoped BaTiO₃ film, was increased with frequency increasing and the dielectric constant was decreased. The possible mechanism of enhanced ferroelectric properties of Fe-doped BaTiO₃ thin film was discussed. The results show the potential role of Fe dopant in improving the ferroelectric properties of BaTiO₃ thin film.