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。     

纳米多孔铝阳极氧化膜的形成机理研究

为探讨多孔铝阳极氧化膜的形成机理,研究了不同气压条件下铝在磷酸溶液中的阳极氧化过程,发现在真空下进行阳极氧化,氧气析出非常明显。通过测定不同气压下的阳极氧化曲线,分析了致密膜向多孔氧化铝膜的转化和生长过程,结果显示氧气析出是导致氧化膜从致密膜向多孔膜转变的主要原因。提出了在氧化膜/电解液界面上氧气分子的聚集是造成表面条纹的新观点。通过氧化膜断面的SEM形貌表征,首次发现多孔膜的主孔道中存在分孔道。分孔道的产生说明析氧反应不但在致密膜/电解液界面发生,而且在多孔膜孔壁/电解液界面也同时发生。     

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.     

甘油对阳极氧化铝纳米孔形成过程的影响

电解电压、电解质种类以及添加剂等因素对氧化铝多孔膜的形成过程有显著影响.在电解液中加入甘油作为添加剂,不但可以增加阳极氧化形成的多孔膜的厚度,而且有利于增强氧化膜的韧性.采用高纯铝作阳极,铂网作为阴极,在草酸溶液中进行恒压阳极氧化.研究了在3%(质量分数)草酸溶液中,添加甘油对氧化铝多孔膜形成过程的影响.结果发现,添加甘油并不会改变氧化铝多孔膜的形成过程,也不会改变形成氧化铝多孔膜中Al2O3的非晶态结构,但甘油的加入将降低阳极氧化时多孔氧化铝膜的生长速度以及氧化铝阻挡层的形成速度,同时增加了纳米孔阻挡层的厚度,因此增加阻挡层的形成时间.在阳极氧化电解液中加入甘油还有利于减小氧化铝多孔膜的纳米孔孔径.     

铝阳极氧化膜的扩孔处理

铝多孔质阳极氧化膜是制备自润滑阳极氧化铝的基础，其技术关键之一是在不破坏氧化膜结构与性能的前提下，尽可能扩大微细孔的孔径。本文用透射电镜（ＴＥＭ）、显微硬度仪、ＳＲＶ摩擦实验机等设备，系统考察了草酸溶液中生成铝阳极氧化膜的微观多孔质结构以及经扩孔处理后该氧化膜多孔质结构的变化和对氧化膜机械性牟的影响，重点探讨了扩孔处理对氧化膜表面硬度和耐磨性的影响，并由此确定了最佳扩孔时间及最佳孔径，为制备纳米量     

预处理工艺对制备多孔阳极氧化铝膜的影响

对铝的预处理工艺进行了研究,详细探讨了高温退火、除油及电化学抛光等对多孔阳极氧化铝形貌的影响.实验结果表明,采用丙酮除油效果最好,不经高温退火和电化学抛光仍能得到高度有序的多孔阳极氧化铝膜,使制备工艺得到了简化.其原因是两步阳极氧化法可以消除铝的内部结构及表面缺陷对多孔氧化铝膜有序性的影响.     

多孔型阳极氧化铝膜在纳米结构制备方面的研究和进展

铝的阳极氧化技术是一种被广泛应用的表面处理方法。近年来，人们发现用这种方法得到的多孔型阳极氧化铝膜（PAA）对于纳米材料的制备有着重要意义。成为国际研究的热点，本文回顾和介绍了铝的阳极氧化技术的机理，工艺和生长规律，介绍了多孔型阳极氧化铝膜在纳米结构制备方面的最新研究进展。     

剧烈-温和阳极氧化结合法快速制备有序阳极氧化铝膜的研究

本研究采用剧烈-温和阳极氧化(hard anodization-mild anodization, HA-MA)结合快速制备高度有序多孔阳极氧化铝(porous anodic alumina, PAA)膜的方法, 即先利用HA在铝表面快速形成有序凹坑阵列, 然后再对表面留有有序凹坑的铝基进行温和阳极氧化, 制备出有序PAA膜。研究了剧烈阳极氧化时氧化电压、氧化时间对所制备PAA膜有序度的影响。研究结果表明, HA-MA结合法制备PAA膜的优化HA参数为: 0.3 mol/L硫酸、80 V、10 min。HA-MA结合法所制备PAA膜的有序性和机械稳定性与二步温和阳极氧化法的相近, 但形成有序PAA膜所需的时间为4.5 h, 约为温和阳极氧化法的1/4, 极大地提高了高度有序PAA膜的制备效率。     

高度有序多孔阳极氧化铝膜形成机理的探讨

使用高纯铝片,利用电化学阳极氧化制备了多孔阳极氧化铝(AAO)膜,用原子力显微镜(AFM)对其形貌进行了表征,提出铝阳极氧化过程中纳米孔从无序到有序的自组织模型,探讨了高度有序六角形纳米孔阵列的形成过程,并分析了影响纳米孔有序度的因素及提高有序度的途径.根据自组织模型探讨了长时间阳极氧化和二次氧化条件下形成高度有序六角形纳米孔阵列的机理.     

多孔氧化铝膜的制备与形成机理的研究概况

直流恒压条件下,酸性溶液中铝的阳极氧化会形成多孔阳极氧化铝(AAO)。其孔径为纳米级且分布均匀,纵横比大,是合成一维纳米材料的理想模板。本文综述了AAO的结构模型、制备方法、形成机理及其应用热点。     

Synthesis of aluminum oxy-hydroxide nanofibers from porous anodic alumina

A novel method for the synthesis of aluminum oxy-hydroxide nanofibers from a porous anodic oxide film of aluminum is demonstrated. In the present method, the porous anodic alumina not only acts as a template, but also serves as the starting material for the synthesis. The porous anodic alumina film is hydrothermally treated for pore-sealing, which forms aluminum oxy-hydroxide inside the pores of the oxide film as well as on the surface of the film. The hydrothermally sealed porous oxide film is immersed in the sodium citrate solution, which selectively etches the porous aluminum oxide from the film, leaving the oxy-hydroxide intact. The method is simple and gives highly uniform aluminum oxy-hydroxide nanofibers. Moreover, the diameter of the nanofibers can be controlled by controlling the pore size of the porous anodic alumina film, which depends on the anodizing conditions. Nanofibers with diameters of about 38-85?nm, having uniform shape and size, were successfully synthesized using the present method.     

The study on oxygen bubbles of anodic alumina based on high purity aluminum

U–t curve has been determined in anodic oxidation of high purity aluminum in two kinds of electrolytes. The formation of the barrier anodic aluminum oxide (AAO) film, the transformation from the barrier film to the porous one and the development of the porous film were analyzed in detail through the SEM micrograph. It was proposed that the porous films have developed from where they used to be seen as the phase of the formation of barrier films. The generation of O₂ in metal/film interface goes with the formation of porous films, so that the AAO film, whether or not it has begun to transform from barrier type to porous type, can be judged by observing if O₂ separates out or not.     

Fast fabrication of long-range ordered porous alumina membranes by hard anodization

Nanoporous anodic aluminium oxide has been widely used for the development of various functional nanostructures. So far these self-organized pore structures could only be prepared within narrow processing conditions. Here we report a new oxalic-acid-based anodization process for long-range ordered alumina membranes. This process is a new generation of the so-called "hard anodization" approach that has been widely used in industry for high-speed fabrication of mechanically robust, very thick (>100 microm) and low-porosity alumina films since the 1960s. This hard anodization approach establishes a new self-ordering regime with interpore distances, (D(int))=200-300 nm, which have not been achieved by mild anodization processes so far. It offers substantial advantages over conventional anodization processes in terms of processing time, allowing 2,500-3,500% faster oxide growth with improved ordering of the nanopores. Perfectly ordered alumina membranes with high aspect ratios (>1,000) of uniform nanopores with periodically modulated diameters have been realized.     

Formation of porous anodic alumina in alkaline borate electrolyte

The growth of porous anodic films at 60 V in an alkaline 0.13 M borax electrolyte at 333 K is examined using sputtering-deposited aluminium substrates, with a fine band of incorporated tungsten tracer. The findings reveal amorphous alumina films containing approximately conical major pores incorporating finer secondary pores, with film thicknesses similar to that of the oxidized aluminium. Further, the distribution of the tungsten tracer within the film is mainly consistent with its expected migration behaviour in anodic alumina. The results indicate that pore development under the present growth conditions is dominated by field-assisted dissolution of anodic alumina, with an efficiency of film growth of about 50%. The findings are in contrast with those of porous anodic films formed in phosphoric acid electrolyte, which are significantly thicker than the layer of oxidized metal.     

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.     

Morphological evolution of porous nanostructures grown from a single isolated anodic alumina nanochannel

Porous anodic aluminum oxide (AAO) membranes have been widely used as templates for growing nanomaterials because of their ordered nanochannel arrays with high aspect ratio and uniform pore diameter. However, the intrinsic growth behavior of an individual AAO nanochannel has never been carefully studied for the lack of a means to fabricate a single isolated anodic alumina nanochannel (SIAAN). In this study, we develop a lithographic method for fabricating a SIAAN, which grows into a porous hemispherical structure with its pores exhibiting fascinating morphological evolution during anodization. We also discover that the mechanical stress affects the growth rate and pore morphology of AAO porous structures. This study helps reveal the growth mechanism of arrayed AAO nanochannels grown on a flat aluminum surface and provides insights to help pave the way to altering the geometry of nanochannels on AAO templates for the fabrication of advanced nanocomposite materials.     

Low cost fabrication of diamond nano-tips on porous anodic alumina by hot filament chemical vapor deposition and the field emission effects

A novel growth method for diamond nano-tips on porous anodic alumina (PAA) by hot filament chemical vapor deposition has been investigated for the first time. Before diamond film deposition could be carried out, nano-diamond particles were deposited onto the pore surface of PAA by electrophoretic deposition at the nucleation sites. Diamond nano-tips were then successfully formed by the shape of porous alumina. The results show that a diamond nano-tip with a smaller radius has superior effects of field emission. Its threshold field and current density are 1.2 V μm(-1) and 4.0 mA cm(-2), respectively, for the case of a tip radius of about 20-30 nm.     

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.