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。     

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.     

Surface morphology control on porous anodic alumina in phosphoric acid

We report the detailed surface morphology control of porous anodic aluminas (PAAs) fabricated in phosphoric acid. The surface defects can be dramatically lessened by employing the second anodization process, but there are still distortions on the surface. In the second anodizing process, the electric field distribution is not regular at the beginning due to the various pore shape and size, which leads to PAA surface distortion. One way to eliminate the surface morphology distortion is to burn the surface defects under higher temperature and higher anodizing voltage, and another way is to have well ordered nanopore array in oxalic acid before anodizing in phosphoric acid to restrict the electric field.     

无阻挡层多孔阳极氧化铝膜板的制备

提出一种在中性的KCl溶液中用多孔阳极氧化铝作阴极,通过电解在阴极产生OH-腐蚀阻挡层,制备无阻挡层氧化铝模板的新方法.用扫描电镜对模板进行了表征.结果表明,在草酸溶液中,制得的氧化铝模板孔径为70～80nm,孔间距为130nm,孔密度约8×109/cm2,这种方法去阻挡层不扩大模板孔径,不影响纳米孔的纵横比.无阻挡层的氧化铝模板适合于直流电沉积和无电沉积金属纳米材料.     

多孔阳极氧化铝模板的制备及其光学特性研究

采用二次阳极氧化法获得分布均匀、有序的纳米多孔阳极氧化铝模板（PAAT），对其形貌、相结构及光学性能进行了表征和分析。光吸收测试发现多孔阳极氧化铝模板在250nm处有一个吸收峰，可见光区是透明的。光致发光测试表明多孔阳极氧化铝模板在450-550nm之间有一个较宽的蓝色发光带，发光峰在460nm左右。     

Magnetic and optical properties of porous anodic alumina/co composite films with gradual microstructures

A simple method to tune the magnetic and optical properties of porous anodic alumina (PAA) films embedded with Co nanowires is reported. The PAA/Co composite films with gradually changing microstructures displayed highly saturated rainbow rings of structural colours and gradual magnetism after being synthesized following a one-step AC electrodeposition method. The magnetization and optical properties of the films can be effectively tuned by varying the deposition voltage, time and controlling the distance between electrodes. A theoretical study on the electrodeposition mechanism that requires gradually changing the length of Co nanowires is consistent with the reported experimental results.     

Reduction of nanoparticle deposition during fabrication of porous anodic alumina

In this paper, we present evidences of nanoparticle deposition on porous anodic alumina (PAA) surface under different anodizing conditions, and discuss the formation mechanism of precipitations. Low-temperature anodization, vigorous stirring and ultrasound-assisted anodization are proposed to reduce the hydrolysis product or hinder its deposition on the surface as well as inside nanopores of PAA. It is discovered that the ultrasound is very efficient to prevent the deposition of Al³⁺ hydrolysis product on PAA. This study is of great value for realizing ordered PAAs with clean surface.     

Comparative study of porous anodic alumina: effects of aluminium deposition methods

This article reports on the comparative study of the fabrication of porous anodic alumina films by anodisation of the aluminium films on glass substrates which were deposited by direct current sputtering and electron beam evaporation methods. The relationship between surface morphology of the deposited aluminum films and porous anodic alumina films was investigated. A more uniform and ordered porous anodic alumina was obtained by fabricating from electron beam evaporation deposited aluminium film with smaller and compact grains. Two-step anodisation was used to further improve the quality of porous anodic alumina compared to one-step anodisation. The optical transmittance spectra within wavelength of 370–800 nm were obtained and the optical properties were studied.     

高度有序多孔阳极氧化铝薄膜光学常数的确定

采用二步阳极氧化法制备了多孔阳极氧化铝(PAA)薄膜,借助于扫描电子显微镜(SEM)分析了多孔阳极氧化铝薄膜的微观形貌,发现在其表面孔径为70～90 nm的六边形孔洞分布均匀,且垂直于表面平行生长.依据PAA反射光谱的实验数据,利用Kramers-Kronig关系计算出PAA薄膜的复折射率、复介电常数以及光学能隙等光学常数.通过分析吸收系数与入射光子能量之间的关系,表明PAA具有直接带隙(能隙约为3.4eV)半导体的光学性质.     

Investigation on highly ordered porous anodic alumina membranes formed by high electric field anodization

A simple and cost effective method for fabricating long-range ordered porous anodic alumina (PAA) membranes is presented, which explores a self-ordering regime with controllable interpore distances over a large scale (300–360 nm). The cohesive force at the hemi-spherical scallop/cell wall (HS/CW) interface is weaker than the other locations. When the PAA membranes were immersed in H₃PO₄ solution, regular cheese-like hexagonal patterns have been propagated at the cell boundaries. With increased etching time, numerous pores were observed at triple points where three cells met. The distinct fracture and etching behaviors in PAA can be ascribed to the intense ionic transport accompanied by the volume expansion in the barrier region under high electric field.     

A simple one-step anodising method for the synthesis of ordered porous anodic alumina

Porous anodic alumina (PAA) has been produced on aluminium substrate by single-step anodising at 50?V in 0.3?M oxalic acid at 15°C for 60?min. The highly ordered pore and cell structure was achieved by subjecting the PAA to oxide dissolution treatment in a mixture of chromic and phosphoric acids. The nanostructure prior and post-oxide dissolution treatment was examined under scanning electron microscope. It was found that the oxide dissolution treatment improves the regularity of the cell and pore structure significantly. Uniform closely packed honeycomb structure of PAA is obtained. The uniformities of pore diameter and interpore distance are also enhanced. Compared to the PAA prior treatment, it was noticed that the pore diameter of the post-treatment PAA increases.     

铝箔表面复合阳极氧化膜研究

采用溶液浸渍法在低压腐蚀铝箔表面沉积一层Ti氧化物．然后将试样在有机盐水溶液中阳极氧化至20．0V。在恒流升压过程中,记录电压-时间曲线。借助XPS和XRD等分析手段分析阳极氧化膜结构,并对复合阳极氧化膜的生长机理进行了探讨。结果表明：含Ti处理液浸渍处理后,试样阳极氧化的电压-时间曲线斜率显著增大,阳极氧化膜是由Al2O3和TiO2构成的复合阳极氧化膜,其介电常数高于Al2O3阳极氧化膜,使阳极箔比容提高24．8％。     

阳极氧化工艺制备氧化铝模板

多孔氧化铝模板是一种用于制作纳米结构材料的模板.为了制作出理想的模板,采用不同的阳极氧化工艺制备多孔氧化铝模板,通过改变工艺参数研究了模板孔径的变化规律,结果表明,在适宜条件下,纳米级氧化铝模板具有六方紧密堆积柱状结构,在每个六棱柱的中心有一个与膜表面垂直的圆柱孔.在一定范围内,随着氧化电压、电流密度、反应温度、铝片纯度的增加氧化铝模板的孔径也随之增加.     

多孔阳极氧化铝膜在纳米功能材料制备中的应用

纳米材料具有一系列不同于块体材料的新异特性，在许多领域都有着广阔应用前景。阳极氧化铝膜具有独特的多孔结构，可作为制备各种纳米功能材料的模板，因而在纳米功能材料制备中占有重要地位。本文综述了多孔阳极氧化铝模板的结构特征、制作方法及由模板合成法制备的多种纳米功能材料的研究与应用现状，并介绍了模板及纳米功能材料的常用表征手段。     

硫酸中阳极氧化制备Al2O3多孔模板的BPANN模拟

采用24组硫酸阳极氧化多孔膜的样本数据建立BP神经网络模型,得到了多孔膜孔有序度与硫酸阳极氧化参数之间的最优关系,经检验该模型的预测结果与实测结果相一致.表明BPANN 是硫酸阳极氧化制备多孔膜孔有序度的较好的预测模型.     

从壁垒型氧化膜生长过程研究PAA的生长机制

为研究PAA的生长机理,设计了铝在3种电解液中的阳极氧化,通过SEM和阳极氧化曲线详细分析了规则圆柱形孔道和表面不规则孔洞产生的原因.电解液中阴离子使氧化膜变成了壁垒层和污染层两层.雪崩电子电流导致了在壁垒层/污染层界面上O2的析出.PAA中圆柱形孔道的形成是氧气析出的结果,传统的"酸性场致溶解"只在表面形成不规则的孔洞.当电解液中磷酸含量减少后,氧气析出持续的时间降低,O2析出停止后,多孔孔道被新生成的氧化铝封堵,最后PAA膜转变成BAA膜.     

Characterization of the anomalous luminescence properties from self-ordered porous anodic alumina with oxalic acid electrolytes

The pore height and diameter of the nanoscale structure of porous anodic alumina (PAA) film produced by the anodization technique are controllable. The structures can be applied for the fabrication of visible spectral range optical devices. In this study we characterized the luminescence properties of self-ordered PAA films evaporated onto silicon substrates. Anomalous luminescence properties produced by carrier confinement were observed in PAA films fabricated with the introduction of oxalic acid electrolytes during the anodization process. The recombination mechanisms were characterized by measuring the temperature-dependent photoluminescence (PL) spectra. The PL spectra of PAA films show an asymmetrical luminescence profile in the blue emission region. The Gaussian function divides these into two subbands. The subbands originate from two different kinds of oxygen-deficient defect centers, namely, F⁺ (oxygen vacancy with only one electron) and F (oxygen vacancy with two electrons) centers. The F centers are densest at the surface but show a gradual decrease with an increase in the pore wall depth and electrolyte concentration. However, the reverse trend is observed for the F⁺ centers. In strong contrast to the commonly expected trend of a uniform reduction in non-radiative recombination with decreasing lattice temperature, we observed an anomalous low-temperature PL growth and decline between the F and F⁺ centers. Theoretical models corroborate the anomalous temperature behavior. All the calculations are in agreement with the experimental observations.     

Mesoporous structures confined in anodic alumina membranes

The synthesis of nanoporous membranes based on different concepts and materials is a field of active research. This review focuses on the synthesis strategies, mesophase evolution mechanisms and potential applications of mesoporous materials confined within anodic alumina membranes (AAM). Following a rapid evolution of synthetic techniques, a significant number of different mesoporous materials (e.g., silica, titania, and carbon) with highly regular structures can now be prepared within these membranes. In recent years, efforts have also been made to understand the formation mechanisms of these hierarchical mesophases. The resulting organized nanoporous membranes open up a wide range of potential applications in fields such as templating oriented nanowires and controlled separation and release of molecules. For example, while various synthesis strategies can be used for the preparation of membrane-embedded nanowires, the latter can also be obtained as isolated objects after dissolution of the alumina host matrix. The review also discusses issues such as control of structural defects or integrity of interfaces that should be addressed in future research in order to fully exploit the potential of these hierarchical mesoporous channel structures.     

Oxygen evolution and porous anodic alumina formation

A new formation mechanism of porous anodic alumina (PAA) is proposed, which emphasizes the close relationship between pore generation and oxygen evolution during aluminum anodization. Two special experiments were designed to confirm the formation mechanism: (1) to introduce a reducing agent in anodization for oxygen suppression, and (2) to perform anodization under a reduced pressure for easy oxygen release. The results showed that both reducing agent and atmospheric pressure had a great effect on the morphology of the resultant film. This can be expected on the basis of our hypothesis about the formation mechanism of PAA, but cannot be easily explained by the existing theories.