Preparation of regularly structured nanotubular TiO2 thin films on ITO and their modification with thin ALD-grown layers

Nanotubular titanium dioxide thin films were prepared by anodization of titanium metal films evaporated on indium tin oxide (ITO) coated glass. A facile method to enhance the adhesion of the titanium film to the ITO glass was developed. An optimum thickness of 550 nm for the evaporated titanium was found to keep the film adhered to ITO during the anodization. The films were further modified by growing amorphous titania, alumina and tantala thin films conformally in the nanotubes by atomic layer deposition (ALD). The optical, electrical and physical properties of the different structures were compared. It was shown that even 5 nm thin layers can modify the properties of the nanotubular titanium dioxide films.     

多彩结构色氧化铝薄膜氧化机制的研究

在草酸电解液中,球形碳点电极作为阴极,铝箔作为阳极,利用一次氧化工艺成功的制备出了单一色彩和虹彩环形结构色的氧化铝薄膜.实验结果显示,球形碳点电极下制备的氧化铝薄膜厚度由薄膜中心向外呈对称性递减.当薄膜的径向厚度差在某一波长光的覆盖范围内时,薄膜呈现单一结构色,而当径向厚度差超出某一波长光的覆盖范围时,薄膜呈现虹彩环形结构色.本文详细的讨论了电极间距、氧化电压和氧化时间对薄膜结构色的影响,并从理论上分析了球形碳点电极下多孔氧化铝薄膜的氧化机制.     

How structure changes in fabrication of large size ordered anodic alumina film?

Large size anodic alumina film has not been used in the industry due to that the fabrication parameters are very difficult to control, but the fabrication of large size anodic alumina is exigent as a template in the fabrication of diverse nano-devices oriented to the industrialization. In this paper, large size (width length = 80 mm × 80 mm) porous ordered anodic alumina film was fabricated by using two-step anodization process as compared to the small size (diameter = 40 mm) anodic alumina film in the structures. Pore size and film thickness of anodic alumina film are strongly related to the size of the anodization film. The large size anodic alumina film has an ideally ordered pattern by applying low voltage. However, with the increase of voltage, the ordered pattern of the PAA films was gradually disrupted, especially in the 70 V due to the local thermal imbalance.     

Effects of thin-film structural parameters on laser desorption/ionization from porous alumina

Nanoporous aluminum oxide layers, grown by anodization of aluminum thin films on glass and then sputter-coated with gold, were used to study the effects of the thin-film structural parameters on laser desorption/ionization (LDI) mass spectrometry (MS) of peptides. Variation of MS signal intensity was examined as a function of alumina pore depth, pore width, and gold layer thickness. Peptide molecular ion intensity was optimal with porous alumina formed from aluminum films of approximately 600-nm thickness; thinner or thicker films gave significantly lower signals. Signals decreased when pore sizes were increased beyond the as-formed width of approximately 100 nm. The MS signal also varied with the thickness of the sputtered gold layer with an optimum thickness being approximately 90 nm. The results of these studies provide values for empirical optimization of LDI MS performance as well as potential clues to the LDI mechanism.     

高度有序多孔阳极氧化铝模板的制备

为了得到纳米孔排列高度有序的多孔阳极氧化铝模板,以0.3 mol·L-1的草酸为电解液研究了模板的制备工艺.采用场发射扫描电子显微镜(FE-SEM)对多孔氧化铝模板的表面形貌进行表征,X射线衍射分析高纯铝及氧化膜的结构.实验结果表明,铝基体不经过高温退火处理,同样能够得到高度有序的氧化铝膜,简化了多孔氧化铝膜的制备工艺.分别讨论了阳极氧化电压和电解液温度对多孔阳极氧化铝膜的形貌及孔径的影响,并对一步法和两步法制得的多孔氧化铝膜进行比较,结果表明,两步阳极氧化法制备的多孔氧化铝模板的有序性优于一步氧化法.XRD分析证实,多孔氧化铝膜由非晶态的Al2O3组成.     

Structural study of very thin anodic alumina films on silicon by anodization in citric acid aqueous solution

The formation of thin alumina films on a silicon substrate by anodization in a mild acid, specifically in 1% wt citric acid aqueous solution, is investigated by transmission electron microscopy (TEM). We present a comparative study between two cases of starting material: pure aluminum and an alloy of aluminum with 1% silicon. In both cases the thickness of the Al layer was less than 50 nm. It was observed that under exactly the same conditions, in the first case the anodization was stopping before anodizing the whole film and a remaining non-anodized Al layer was always present, while in the second case, the Al layer was fully anodized, resulting in an alumina matrix with a very high density of silicon nanocrystals of uniform sizes embedded in it. In both cases the alumina film was compact and amorphous.     

Nanopatterned silicon emitters of a solar cell fabricated by anodic aluminum oxide masks

We investigated the nanopattern transferring process by a template of anodic aluminum oxide and the formation of a nanoporous aluminum oxide layer on a Si solar cell by the anodization process of Al thin films. The anodization process provided a template to transfer the nanopattern onto the Si surface. The small-sized nanoporous alumina template was attached to be covered on the textured surface and played the role of etching mask in the F-based dry etching process. Furthermore, we deposited an Al thin film onto the Si surface and the subsequent anodization process was performed. The alumina formulated on the deposited Al thin film did not show the array of nanoporous structure and no nanopatterns were transferred onto the surface. The large-areal alumina deposited on the Si surface showed enhanced photo-absorption in the ultraviolet spectral region of 243 nm, but increased the photo-reflectance in the visible and infrared spectral regions when compared to the Si-bare sample.     

Effects of composition and thickness on the electrical properties of indium oxide/tin oxide multilayered films

Indium oxide/tin oxide multilayered films with a 2 nm pair thickness were deposited on glass substrates at temperatures lower than 100° C by an ion-beam sputtering method. The structure, electrical properties and visible transmissivity were investigated as a function of composition and the total thickness on as-deposited and annealed films. X-ray diffraction analysis showed that the as-deposited 200 nm thick film (with 0.15 nm tin oxide layers) was partially crystalline and films thinner than 100 nm were amorphous or microcrystalline. The roomtemperature resistivity of as-prepared films increased with the increase of an average tin oxide layer thickness from ∼0.05 to ∼0.3 nm (ideal monolayer thickness) under a constant total thickness ∼100 nm. We observed a decrease of the Hall mobility with the increase of the total film thickness from 10 to 200 nm in as-deposited samples containing 0.15 nm tin oxide layers.     

壁厚不连续不对称圆柱壳和开口壳的自由振动分析

视壁厚不连续不对称的圆柱壳或开口壳为层合壳。以弹性力学中的Hamilton正则方程为基础,分别应用Hamilton正则方程的半解析法构建层合壳每一层的线性方程。考虑到每两层连接界面上应力和位移的连续性,联立各层的方程得到系统的控制方程和特征方程。主要的优点是系统的控制方程不限制圆柱壳的厚度,数学模型和数值方法也适应分析壁厚不连续且壁厚不对称的复合材料层合壳问题。     

Inside Front Cover: Fabrication of Ideally Ordered Nanoporous Alumina Films and Integrated Alumina Nanotubule Arrays by High‐Field Anodization (Adv. Mater. 17/2005)

A simple, low‐cost approach to fabricating large‐area highly ordered nanoporous alumina films in sulfuric acid solutions through a single‐step high‐field anodization, without the assistance of any additional process, is reported on p. 2115 by Chu and co‐workers. The critical high anodizing potential in the adopted electrolyte system increases with the ageing of solutions after a long period of anodization. Correspondingly, the applicable current density for stable anodization rises significantly, thus leading to high‐speed film growth. Uniform porous anodic alumina films in sulfuric acid solutions under a high electric field of 40–70 V and 1600–2000 A m^–2 are achieved.     

Magnetic properties of permalloy/permalloy-oxide multilayer thin films

Magnetic properties of permalloy/permalloy-oxide multilayer thin films are investigated. These thin films are prepared by a repeat of sputter deposition of permalloy thin film, followed by oxidation of the film surface. The total thickness of the permalloy thin films before oxidation is about 100 nm. The number of layers is one to twenty. The oxide layers are formed by oxidation in dry air. The estimated oxide layer thickness is about 2 nm. The oxide NiFe₂O₄ is identified by RHEED. The film coercivity decreases linearly with increasing layer numbers. The saturation magnetization and magnetoresistivity decrease as the number of layers increase. The coercivity decrease is due to grain growth suppression and magnetic separation by oxide film of permalloy layer, and magnetoresistivity decrease is due to electrical resistivity increase originating into electron scattering by the oxide layer.     

Controlled fabrication of patterned lateral porous alumina membranes

Confined lateral alumina templates are fabricated with different pore sizes by changing the acid electrolyte and the anodization voltage. The control of the number of pore rows down to one dimension is also achieved, by controlling the thickness of the starting aluminum film as well as the anodization voltage. We observe that the mechanism of pore formation in the lateral regime is very similar to that in the classical vertical situation.     

Computational approach of piezoelectric shells by the GDQ method

A piezoelectric laminated cylindrical shell with shear rotations effect under the electromechanical loads and four sides simply supported boundary condition was studied by using the two-dimensional generalized differential quadrature (GDQ) computational method. The typical hybrid composite shells with 3-layered cross-ply [90°/0°/90°] graphite–epoxy laminate and bounded PVDF layers are considered under the sinusoidal pressure loads and electric potentials on the shell. The governing partial differential equation with first-order shear deformation theory in terms of mid-surface displacements and shear rotations can be expressed in series equations by the GDQ formulation. Thus we obtain the GDQ numerical solutions of non-dimensional displacement and stresses at center position of laminated piezoelectric shells. Displacement is generally affected by the thickness of laminated piezoelectric shells under the action of mechanical load. Stresses are generally affected by the thickness and the length of laminated piezoelectric shells under the actions of mechanical load and electric potential.     

Craze yielding and fracture mechanism in PE/PS/PE laminated films

The change in polystyrene (PS) layer thickness, which has been simultaneously determined during post-yield deformation, shows that crazing is the basic mechanism of toughening in all laminated films, and that shear deformation supplements the contribution of crazing especially for samples with high polyethylene (PE) volume fractions. Crazes formed in PS layers in the laminated films are slender and regular compared with the short and lenticular crazes formed in bulk PS film. When PE volume fraction increased, craze advance speed decreased because of the reduction of the stress concentration effect at craze tips. The life-time of the first mature craze to be formed at a given strain rate increased with PE volume fraction because the PE supporting the mature crazes could effectively inhibit craze rupture and blunt out the propagating crack by absorbing the stored elastic energy in the PS layer that would have been dissipated as fracture surface energy.     

两步阳极氧化法制备多孔阳极氧化铝膜

直流恒压下,在酸性溶液中对铝实施两步阳极氧化制备了多孔氧化铝膜。采用扫描电镜(SEM)、原子力显微镜(AFM)对制备的多孔氧化铝膜进行形貌分析,孔径在纳米级且孔分布具有高度均匀性。采用SEM对试样进行观察,分析了工艺对多孔氧化铝膜形貌的影响。利用阳极氧化初期电流密度的变化并结合阳极氧化过程中的试样的SEM照片,分析了多孔氧化铝膜的形成机理。     

Improvement in corrosion resistance of NiTi by anodization in acetic acid

NiTi was galvanostatically anodized in acetic acid to increase the oxide film thickness for improving corrosion resistance. The galvanostatic anodization behavior of NiTi in acetic acid differed markedly from that of Ti. In particular, the anode potential reached was much lower for NiTi, and thus only thin oxide films could be obtained. With a suitable choice of anodizing conditions, the anodic oxide film formed had a thickness of 20–25 nm, as determined by profilometric measurement. Atomic force microscopy (AFM) revealed that the surface roughness was increased after anodization. Analysis by X-ray photoelectron spectroscopy (XPS) showed a low Ni/Ti ratio of 0.04 at the anodic oxide surface versus a value of 0.30 for bare NiTi. Electrochemical impedance measurements of the anodized sample in Hanks' solution at 37 °C recorded a 9-fold increase in polarization resistance, and cyclic polarization tests also recorded a matching reduction in the passive current density. These observations indicate that anodization of NiTi can serve as a simple low-temperature method to enhance the corrosion resistance of NiTi when used as an implant material.     

高电压下多孔氧化铝薄膜结构色的制备及分析

多孔氧化铝的微观结构对其光学性能有着显著影响.本文采用高电压制备了普通阳极氧化铝薄膜(单层薄膜)和经高电压表面处理后的光子晶体(多层薄膜),通过理论分析,并结合扫描电镜分别对两种环形氧化铝薄膜建立了微观结构模型图.研究表明:在磷酸电解液中,使用一步阳极氧化方法制备的普通阳极氧化铝多种环形结构色,从中心到边缘结构色逐渐蓝...     

厚度不连续悬臂梁板的自由振动分析

将厚度不连续梁板视为层合板, 分别应用Hamilton 正则方程半解析法建立每一层的线性方程。考虑到每两层连接界面上应力和位移的连续性, 联立各层的方程得到整个结构的特征方程, 其主要的优越性表现为: 控制方程不限制不连续梁板的厚度, 并能适合处理厚度不对称且不连续的层合板。本文中的方法可修改或扩展用来分析加筋压电材料层合板或带有压电材料传感器和驱动器块的板壳等问题。      

Free Vibration of Laminated Composite Shallow Shells Containing Piezoelectric Layers

The free vibration of laminated shallow shells containing piezoelectric layers is investigated in this article. A finite-element formulation based on the transverse shear deformation theory has been used to determine the natural frequencies, mode shapes, and modal voltages of laminated composite shell structures containing piezoelectric layers. Comparisons of degenerate cases with published results show excellent agreement. The effect of electromechanical coupling on the predicted natural frequencies is discussed. Results are presented for different geometries, laminate configurations, and boundary conditions. The effects of shell shallowness and piezoelectric layer thickness are also studied. Higher natural frequencies are obtained when the full electromechanical coupling is considered. It is also found that the natural frequencies increase considerably with the shell curvature, particularly for thin piezoelectric layers.     

Structural engineering of nanoporous anodic aluminium oxide by pulse anodization of aluminium

Nanoporous anodic aluminium oxide has traditionally been made in one of two ways: mild anodization or hard anodization. The first method produces self-ordered pore structures, but it is slow and only works for a narrow range of processing conditions; the second method, which is widely used in the aluminium industry, is faster, but it produces films with disordered pore structures. Here we report a novel approach termed "pulse anodization" that combines the advantages of the mild and hard anodization processes. By designing the pulse sequences it is possible to control both the composition and pore structure of the anodic aluminium oxide films while maintaining high throughput. We use pulse anodization to delaminate a single as-prepared anodic film into a stack of well-defined nanoporous alumina membrane sheets, and also to fabricate novel three-dimensional nanostructures.