铝电化学阳极氧化技术研究进展

深入探讨了铝阳极氧化膜的形成机理和结构特征,阐述了铝多孔氧化膜形成过程的主要影响因素;说明了不同氧化工艺参数下的膜形貌,介绍了铝多孔氧化膜独特的结构在功能材料上的应用状况和发展前景,并提出了氧化膜的发展趋势。     

Al2O3纳米线薄膜的制备及其生成机理研究

研究了一种简单新颖的制备Al2O3纳米线薄膜的电化学方法。以阳极氧化法在高纯铝片表面制备多孔阳极氧化铝的工艺为基础,在草酸电解液中通过一次阳极氧化过程,将阳极氧化铝孔壁溶解形成Al2O3纳米线,均匀覆盖在阳极氧化铝有序孔道的上方,得到一种特殊结构的纳米线薄膜。使用扫描电镜、高分辨透射电镜和X-射线能谱仪对纳米线的形貌、结构及成分进行了表征分析。并结合扫描电镜对不同反应时间长度的产物形貌来观察纳米线的生成过程。探讨了Al2O3纳米线薄膜的生成机理。     

纳米氧化铝模板(AAO)的制备

多孔性阳极氧化铝(AAO)模板具有制备容易、成本低、孔道分布均匀等特点,是制备纳米材料的理想无机模板,近几年颇受人们的关注,获得了深入的研究。本文介绍了在草酸和磷酸溶液中,制备纳米氧化铝模板的阳极氧化工艺以及不同的电解液对模板特性的影响,并用扫描电子显微镜(SEM)对阳极氧化铝膜的形貌和结构进行了表征。     

载银抗菌新型铝材料的研制

在经过阳极化处理的铝板表面采用吸附、电沉积的方法,将金属银沉积于氧化膜的微孔中,并利用金相显微镜观察了形成的载银材料表面的情况,对不同的沉积条件下生成的材料进行了分析讨论。结果表明,在AgNO3溶液电沉积过程中,加入适量的保护剂,可以使沉积在铝板表面及氧化膜微孔中的银颗粒粒径变小,分布均匀,提高载银铝材料的表面性能。     

电流密度对5252铝合金阳极氧化膜性能的影响

以5252铝合金阳极氧化膜为研究对象,研究了电流密度对阳极氧化膜性能的影响,以及阳极氧化处理后铝材表面产生"粉化"缺陷的机制。结果表明:阳极氧化膜的厚度随电流密度的增加先增大后减小,当电流密度为2.41 A/dm²时阳极氧化膜的厚度达到最大值32.2μm。随着电流密度的增加,阳极氧化膜的显微硬度逐渐降低,这主要是由阳极氧化膜的孔径和孔隙率增大造成的。另外,阳极氧化处理后铝材表面产生"粉化"现象。这主要是因为阳极氧化膜表面的孔隙率增加,孔的连续性分布变差。     

Bonding properties between nitrile–butadiene rubber and aluminum alloy treated by anodizing methods

In this work, the bonding properties between the LD7 aluminum alloy anodized by sulfuric acid or phosphoric acid and nitrile–butadiene rubber (NBR) were investigated. The bonding properties between the anodized aluminum alloys and NBR were compared with those between aluminum alloys treated by burnishing or sandblasting and NBR. The results revealed that, in comparison with sulfuric acid anodized samples, samples anodized in phosphoric acid solutions showed higher 90° peel strength. Under the same conditions, an increase in the anodic film thickness in the studied range may improve the adhesion property between rubber and an aluminum alloy. In comparison with aluminum alloys treated by burnishing or sandblasting, the surface of the anodized aluminum alloy showed homogeneously dispersed pores, which resulted in better and homogeneous bonding properties. A vacuum‐drying process on the anodized aluminum alloys after they were coated with adhesives facilitated penetration of the adhesive molecules into the pores on the oxide layer, which considerably improved the bonding properties. In addition, rubber macromolecules could also penetrate the pores in the aluminum oxide layer, leading to a strong physical anchor–hold interaction after a long time of soaking and diffusion. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

电压对7N01铝合金阳极氧化膜结构及耐蚀性的影响

采用160 g/L硫酸溶液在17℃下对7N01铝合金阳极氧化30 min,氧化电压分别选取14、15、16、17和18 V。用扫描电镜观察所得阳极氧化膜的形貌,用能谱仪和电化学测量分析了它的成分、厚度和耐蚀性。结果表明,7N01铝合金经过不同电压下的阳极氧化处理后,表面均能形成凹凸不平并有孔洞的阳极氧化膜,电压为17 V时所制膜层致密、均匀,厚度约为7.6μm,耐蚀性最佳,在3.5%NaCl溶液中浸泡1 440 h后没有明显的腐蚀。     

Features of the formation of nanoporous membranes based on alumina from foil and new fields of applications

The peculiarities of the formation of porous membranes based on aluminum oxide obtained by the electrochemical anodization of aluminum foil with the preset topological parameters of pores-capillares (20–220 nm) have been studied. The methods to study the membranes based on nanoporous aluminum oxide are proposed. The developed nanoporous material possesses the properties of screening IR radiation in a spectral range of 8–14 μm (corresponds to the spectral region of thermal radiation of bioobjecs). The membranes based on anodized aluminum foil provide the fulfilling the functions of channeling a high-flow helium ions with an energy of 1.5–2 MeV with the experimentally found coefficient of transmission of more than 60%.     

Fabrication of three-dimensional platinum microstructures with laser irradiation and electrochemical technique

Three-dimensional (3D) platinum microstructures were fabricated by successive procedures: aluminum anodizing, laser irradiation, nickel/platinum electroplating, and removal of the aluminum substrate, the oxide films, and the nickel metal layer. Aluminum plates and rods were anodized in an oxalic acid solution to form porous type oxide films. The anodized specimens were immersed in a nickel electroplating solution, and then irradiated with a pulsed Nd-yttrium aluminum garnet (YAG) laser beam to remove the anodic oxide film with a three-dimensional XYZθ stage. The specimens were cathodically polarized in the nickel and a platinum electroplating solution to form the metal micropattern at the laser-irradiated area. The electroplated specimens were immersed in NaOH solution to dissolve the aluminum substrate and the oxide films, and then immersed in HCl solution to dissolve the nickel deposits. A platinum grid-shaped microstructure, a microspring, and a cylindrical network microstructure with 50-100 μm line width were obtained successfully.     

FT-IR Microscopy Studies of Water Ingress into Aluminum-Adhesive Joints

FT-IR microscopy of the effect of humidity on epoxy thin films on anodized aluminum surfaces was performed in the absence of external stress. The oxide transformation was observed in the anodized samples. Moisture damage was greater in the untreated aluminum samples indicating that interfacial debonding occurs faster in these samples. Water damage was localized spatially. The only organic reaction seen was at the epoxy/air interface giving carboxylates at the surface.     

阳极氧化铝的表面参数对硅酮结构的装锒密封胶长期黏结性的影响(连载一)

硅酮密封胶对阳极氧化铝的黏结质量千差万别.影响黏结性的关键因素是铝材表面的封孔程度、氧化层的着色情况、清洁剂的特性以及基材表面清洁与打胶之间允许的时间间隔.由于清洁剂将有机污染物从阳极氧化铝表面去除的效果不同,所以此效果并不和黏结质量有必然联系.据猜测,吸附在阳极氧化铝表面的清洁溶剂会改善基材表面从而提高硅酮胶的黏结性,但这种改善效果会随着清洁溶剂随时间的的挥发而降低.对于给定的溶剂,最佳的黏结效果取决于材料表面的封孔程度.依照ISO 2143酸刻蚀方法测量材料表面的封孔程度,可以预测未着色的阳极氧化铝基材的黏结性.对于着色的阳极氧化铝表面,依照ISO 2931的测试标准,用电相位漂移方法可以用来预测黏结质量.一种控制阳极氧化铝表面的方法被提了出来,此方法是测量不同频率下基材的电阻抗并将它成功地和硅酮密封胶与该材料表面的长期黏接性联系起来.     

Formation of Al2O3–Nb2O5 composite oxide films on low-voltage etched aluminum foil by complexation–precipitation and anodizing

Niobium pentaoxide (Nb₂O₅) thin films were deposited on etched aluminum foils by complexation–precipitation followed by heat treatment. Then the Al₂O₃–Nb₂O₅ (Al–Nb) composite oxide films were formed by anodizing to increase the capacitance of anodized aluminum foils which are used in aluminum electrolytic capacitors. The composition and structure of niobium deposition layer were characterized by X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD), and the microstructures and dielectric properties of anodic oxide films were investigated by scanning electron microscope (SEM) and electrochemical impedance spectroscopy (EIS) respectively. The results show that the niobium deposition layer after heat treatment existed in the form of crystalline Nb₂O₅. The aluminum foil with Nb₂O₅ coating can be anodized with higher efficiency and energy saving. Compared with that of normal anodized aluminum foils, the effective area of the anodized aluminum foils with Al–Nb composite oxide films had no apparent change. The specimens with Al–Nb composite oxide films anodized at 30 V exhibited about 20% higher specific capacitance than that of those with pure aluminum oxide films. It suggests that the method of complexation–precipitation is an effective way to increase the specific capacitance of anodized aluminum foils used in aluminum electrolytic capacitors.     

Synthesis and Study of a Polypyrrole–Aluminum Oxide Nanocomposite Film on an Aluminum Surface

Using the method of electrochemical anodization, aluminum oxide porous films are obtained in a sulfuric acid solution. The morphology of the aluminum oxide surface is studied by the method of scanning electron microscopy. The high-quality elemental analysis of the initial and oxidized Al films is performed using the method of electron microprobe analysis. A protective composite polypyrrole-aluminum oxide film is produced on the aluminum surface on top of a porous aluminum oxide film in the galvanostatic oxidation mode by the electrochemical synthesis method. The properties of the polypyrrole–aluminum oxide composite film are studied by the methods of voltammetry, as well as impedance and FTIR spectroscopy.     

Fabrication and centeracterization of ordered CuIn(1?x)GaxSe2 nanopore films via template-based electrodeposition

Ordered CuIn_(1−x)Ga_xSe₂ (CIGS) nanopore films were prepared by one-step electrodeposition based on porous anodized aluminum oxide templates. The as-grown film shows a highly ordered morphology that reproduces the surface pattern of the substrate. Raman spectroscopy and X-ray diffraction pattern show that CIGS nanopore films had ideal chalcopyrite crystallization. Energy dispersive spectroscopy reveals the Cu-Se phases firstly formed in initial stage of growth. Then, indium and gallium were incorporated in the nanopore films in succession. Cu-Se phase is most likely to act as a growth promoter in the growth progress of CIGS nanopore films. Due to the high surface area and porous structure, this kind of CIGS films could have potential application in light-trapping CIGS solar cells and photoelectrochemical water splitting.     

A study of the adhesion of polyethylene to porous alumina films using the scanning electron microscope

An adhesive bond was formed by sintering low-density polyethylene onto aluminum with a porous anodic film. The topography of the polymer surface in contact with the anodized aluminum was studied in a scanning electron microscope, having removed the aluminum and alumina by dissolution in aqueous sodium hydroxide. The surface of the polymer appeared very rough with large projections of various forms, all of which were many times larger than the pores revealed in the anodic films by transmission electron microscopy. These projections are shown to consist, most probably, of “stacks” or “tufts” of much smaller polyethylene fibers, each of which had entered a pore in the anodic film. Thus, the scanning electron-microscopic investigation confirms the keying mechanism for the adhesionof polyethylene to porous anodic films on aluminum proposed in an earlier paper.     

不同电解质制备多孔阳极化Al2O3的形貌与间接诱导形成钙磷涂层能力

利用在Na3PO4液中的直流恒压阳极氧化法和H3PO4液中的恒流阳极氧化法对纯铝片进行阳极化处理。用扫描电子显微镜观察经阳极氧化样品的形貌结构,电子能谱测定诱导生成钙磷涂层的元素构成。结果表明：Na3PO4电解液中阳极化铝片发生过氧化行为形成过氧化膜;以稀H3PO4为电解液制得了孔径可达120～150nm的规整多孔阳极氧化铝(anodic aluminum oxide,AAO)膜。经多步预处理后．再在模拟体液中浸渍2．5d,过氧化AAO膜比规整多孔AAO膜显示出更为优异的诱导生成钙磷陶瓷涂层的能力。     

Wettability of porous two‐dimensional ZnO nanocrystal films

Large‐scale two‐dimensional ZnO nanocrystal films on aluminum substrate were fabricated by a one‐step hydrothermal method under mild conditions, where all the ZnO nanocrystals had a lamellar structure generally perpendicular to the substrates and formed network‐like porous configurations. The morphologies of the films were dependent on both the reaction temperature and concentration of zinc. The wettability of the ZnO films was assessed by measuring the water contact angle without any surface functionalisation. The porous structures of the as‐prepared films could effectively enhance its hydrophobicity and the water contact angle ranged from 40° to 135° depending on the surface morphology and the arrangement of ZnO planes, indicating a simple and promising route to make aluminum surface waterproof and even self‐cleaning. The hydrophobic ZnO surface could be switched to hydrophilic state by UV irradiation.     

Synthesis and optimization of porous anodic aluminum oxide nano-template for large area device applications

A simplified anodized aluminum oxide (AAO) nano-template fabrication process was developed in this study, which can be suited for the large area device applications. The pores of various sizes and depths were realized from the thin (less than 1 μm) aluminum film deposited on the sapphire substrate. The optimum morphological structure was obtained by adjusting the applied voltage, types of acid solution, its concentration and temperature which has evolved after two phases of anodization followed by chemical etching. The Ar plasma pre-treatment method was developed and applied to improve the surface roughness of thin aluminum film without severely sacrificing the deposited layer thickness.     

汽车用2024铝合金阳极氧化膜性能的研究

对汽车用2024铝合金板材进行酒石酸阳极氧化处理,并研究了阳极氧化对铝合金的成分、结构、表面形貌及耐蚀性的影响。研究发现,铝合金阳极氧化膜是由表面多孔层和内部无孔层构成的。铝合金阳极氧化过程是一个氧化铝生成和溶解的动态过程。阳极氧化膜由刚玉结构的α-Al_2O_3和八面结构的γ-Al_2O_3构成,α相和γ相大大提高了阳极氧化膜的硬度和耐蚀性。阳极氧化膜为典型的多孔结构,孔洞分布均匀,孔径为50nm左右。     

Characterization and Optical Properties of the Single Crystalline SnS Nanowire Arrays

The SnS nanowire arrays have been successfully synthesized by the template-assisted pulsed electrochemical deposition in the porous anodized aluminum oxide template. The investigation results showed that the as-synthesized nanowires are single crystalline structures and they have a highly preferential orientation. The ordered SnS nanowire arrays are uniform with a diameter of 50 nm and a length up to several tens of micrometers. The synthesized SnS nanowires exhibit strong absorption in visible and near-infrared spectral region and the direct energy gap E _g of SnS nanowires is 1.59 eV.