氧化铝阵列模板制备及其影响因素研究

经预处理的铝箔,分别以不同浓度硫酸和草酸为电解液,在不同阳极氧化时间、电压下,用二步阳极氧化法制备多孔有序阳极氧化铝阵列模板,用透射电镜对其形貌和结构进行了表征,用测厚仪测量了氧化膜厚度.研究结果表明,电解液种类、阳极氧化时间、电压等因素对氧化铝阵列模板外观、膜厚、孔径、孔排列有序度都有不同程度的影响.     

结构调制型氧化铝模板的制备及表征

采用两种不同方法制备了结构调制的多孔氧化铝(AAO)模板,一种是磷酸扩孔法,另一种是非对称阳极氧化法。磷酸扩孔法是根据传统有序氧化条件,在模板二次阳极氧化后,用磷酸对已形成的孔道进行扩孔,然后再进行第三次阳极氧化;非对称阳极氧化法是在第一次氧化后形成的有序凹痕上,在始终保持氧化电压与第一次氧化时相同,同时确保相邻两次氧化在不同类型电解液中进行的条件下,制备出孔间距相同、孔径不同的有序结构调制的AAO模板。这些方法扩展了在给定电解液中制备AAO模板的孔径,从而实现了AAO模板的结构调制。     

超声波辅助扩孔对氧化铝模板结构的影响

在0.3mol/dm3的草酸溶液中,采用二次阳极氧化法制备多孔氧化铝模板,研究了阳极氧化后的扩孔处理对多孔膜形貌和结构的影响.SEM和FE-SEM结果表明,经20min超声波扩孔处理后,多孔氧化铝模板纳米孔的结构更加趋于规则,表观孔径从30nm增大到70nm,其扩孔效果较常规扩孔方法更为明显.超声波扩孔时间增加到40min后,多孔膜孔径扩大至100nm,但某些区域的纳米孔壁已被部分溶解.在一定的电压范围内,随着电压增加,经超声波扩孔后的多孔氧化铝膜孔径增大,有序度有较大提高.     

多孔阳极氧化铝微孔结构的调控

多孔阳极氧化铝(AAO)是一种在酸性电解液下,通过施加电压对金属铝阳极氧化获得的多孔膜材料。AAO在当今纳米材料领域有着非常多的应用,如制备纳米阵列、进行纳米复制、制备量子点等。本文采用二次氧化法制备了AAO模板,研究了硫酸、草酸两种电解液以及氧化电压对纳米孔的影响规律。采用扫描电子显微镜(SEM)对样品的表面形貌进行分析,研究了制备工艺对孔形态的影响。通过统计不同氧化电压下AAO孔的圆度和孔径的分布,发现圆度随着电压的升高而升高。孔径随电压的升高而增大,两者呈现成指数型关系。     

长程有序纳米孔氧化铝模板的制备与研究

以硫酸和草酸溶液为电解液,采用二次阳极氧化法制备出高度长程有序的纳米孔氧化铝(AAO)模板,并结合扫描电子显微镜(SEM)对其微观结构及形貌进行了观察和表征.通过研究不同的氧化电压和电解液浓度对AAO模板纳米孔形貌(孔径、孔间距、面密度和长程有序性)的影响,得到了最佳的氧化电压和电解液浓度.     

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.     

AAO模板快速制备方法探究

为了快速制备出高度有序且孔径可调控的AAO(阳极氧化铝)模板应用于工业生产,通过改进传统的两步阳极氧化法,采用逐步提高电解液浓度的硬氧氧化法制备了AAO模板,并确定了最佳制备工艺为初始电解液浓度0.15mol/L,添加电解液浓度0.40mol/L,温度保持在5℃左右,无水乙醇添加比例为1:1,从而使铝片的击穿电压从40V上升到130V左右(模板面积1.5cm×4.5cm),采用DimensionEdge型号的原子力显微镜(AFM)对多孔氧化铝模板进行了表征。结果表明:未经退火处理的铝片,也可以制备出高度有序的AAO模板,但其粗糙度略有增加,并与在高压条件下二次氧化、三次氧化、四次氧化制备AAO模板进行了比较,发现二次氧化制备的AAO模板有序度、孔径、孔间距均优于三次、四次氧化法。     

多孔氧化铝模板的制备研究

以草酸为电解液,采用二次阳极氧化法制备多孔有序氧化铝模板,研究了氧化电压、电解液浓度、去一次氧化膜时间和二次阳极氧化时间对多孔氧化铝膜结构的影响。结果表明,退火后在60V电压、0.6mol/L的草酸溶液中、去一次阳极氧化膜5h、二次阳极氧化15h制备的膜结构孔洞均匀有序、孔径达80nm、孔密度达8.2×109个/cm2。     

泡沫铝合金阳极氧化工艺研究

以草酸为电解液,对泡沫铝合金材料进行阳极氧化处理,制备多孔有序阳极氧化铝阵列模板,采用SEM扫描电镜对其形貌进行分析.研究了电流密度、电解液浓度、电解温度等条件对氧化铝膜结构的影响,并对一步法和两步法制得的多孔氧化铝膜进行了比较,结果表明,氧化膜上的微孔分布均匀,孔径大小基本相同;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.     

多孔氧化铝模板的制备研究

以草酸为电解液，采用二次阳极氧化法制备多孔有序氧化铝模板，研究了氧化电压、电解液浓度、去一次氧化膜时间和二次阳极氧化时间对多孔氧化铝膜结构的影响。结果表明，退火后在60V电压、0．6mol／L的草酸溶液中、去一次阳极氧化膜5h、二次阳极氧化15h制备的膜结构孔洞均匀有序、孔径达80nm、孔密度达8．2×10^9个／cm...     

Effect of process parameters on growth rate and diameter of nano-porous alumina templates

Anodic aluminium oxide (AAO) template with hexagonal shaped nano-pores with high aspect ratio was fabricated by two-step anodization processes from high purity aluminium foil. It was observed that pore dimensions were affected by anodizing voltage, electrolyte temperature and the duration of anodization time. The vertical growth rate of the pores (10?C250?nm/min) was found to vary exponentially with anodizing voltage; however, it exhibits linear increment with the electrolyte temperature. The measured pore diameter (50?C130?nm) shows a linear variation with anodizing voltage. The bottom barrier oxide layer was etched out by pore widening treatment to obtain through holes.     

A Simple Route to Fabricate Percolated Perpendicular Magnetic Recording Media

A simple approach is proposed for fabrication of percolated perpendicular media (PPM). Nano pore array with pore diameter of 12-15 nm and different pore densities has been prepared by anodizing aluminum on silicon wafers. The pore density increases from 3.2times10¹⁰ cm^-2 to 11.0times10¹⁰ cm^-2 with the decrease in anodizing voltage from 30 to 10 V. Then, Pt (7 nm)/{Co (0.5 nm)/Pt (2) nm}₅ multilayers are deposited onto this porous anodized alumina (AAO) by sputtering. The pore size is reduced to 10-12 nm after deposition of magnetic layers. The Co/Pt multilayers on AAO exhibit perpendicular magnetic anisotropy, squareness ratios of unity, and negative nucleation fields. The perpendicular coercivity increases linearly with the increase in pore density due to the pinning effect imposed by the pores, which is consistent with theoretical calculation for PPM     

铝箔多孔阳极氧化铝膜的低温制备及其电化学性能

以多孔阳极氧化铝(AAO)膜制备纳米材料时降低AAO膜孔径至关重要,降低电压无法达到要求,而降低氧化温度可实现这一目标。在0.4 mol/L H3PO4溶液中加入70%～80%(体积分数)1,3-丙三醇(PDO),于-10～10℃下恒压110 V阳极氧化1 h制备了多孔阳极氧化铝(AAO)膜,并在0.50 mol/L H3BO3和0.05mol/L Na2B4O7溶液中于20℃下以0.5 mA/cm2进行填孔后处理。利用SEM,EDS,XRD分析了AAO膜的表面形貌与组成,并对AAO膜填孔前后的极化曲线和交流阻抗谱进行了测试。结果表明,膜孔径随氧化温度降低而降低,80%PDO,10℃所得AAO膜的成分包括65.94%(质量分数,下同)Al,12.79%C,20.29%O和0.98%P;随氧化温度升高和PDO含量下降,AAO膜的稳定电流密度增大;随氧化温度升高,膜阻挡层厚度增大;填孔试验前AAO膜只存在一个阻挡层的相位角峰,填孔后出现两个峰,中高频段体现封闭的阻挡层特性,低频段体现的是多孔层封闭部分的特性。     

Formation of square matrix pores on Al film utilizing focused ion beam milled indent

We successfully fabricated a square pattern of anodic alumina oxide (AAO) template in thin Al film grown on Si substrate utilizing focused ion beam (FIB) milled indent. The pore size and its period of the square matrix were about 50 nm and 100 nm, respectively. We found that the minimum indented depth is required to satisfy the critical electric field which is a vertical component toward downward. In addition, we found that the anodizing voltage plays an important role in determining the pore shape and uniformity. The higher anodizing voltage not only reduces the minimum indent depth that is required to create a matrix array but also improves the uniformity of pore shapes in the matrix array.     

Penetrating the oxide barrier in situ and separating freestanding porous anodic alumina films in one step

A simple method for penetrating the barrier layer of an anodic aluminum oxide (AAO) film and for detaching the AAO film from residual Al foil was developed by reversing the bias voltage in situ after the anodization process is completed. With this technique, we have been able to obtain large pieces of free-standing AAO membranes with regular pore sizes of sub-10 nm. By combining Ar ion milling and wetting enhancement processes, Au nanowires were grown in the sub-10 nm pores of the AAO films. Further scaling down of the pore size and extension to the deposition of nanowires and nanotubes of materials other than Au should be possible by further optimizing this procedure.     

Reduction of interpore distance of anodized aluminum oxide nano pattern by mixed H3PO4:H2SO4 electrolyte

A self-formed and ordered anodized aluminum oxide (AAO) nano pattern has generated considerable interest in both scientific research and commercial application. However, the interpore distance obtainable by AAO is limited by 40-500 nm depending on electrolyte and anodizing voltage. It's believed that below-30 nm AAO pattern is a key technology in the fabrication semiconductor nano structures with enhanced quantum confinement effect, so we worked on the reduction of interpore distance of AAO with a novel electrolyte. AAO nano patterns were fabricated with mixed H2SO4 and H3PO4 as an electrolyte for various voltages and temperatures. The interpore distance and pore diameter of AAO were decreased with reduced anodizing voltage. As a result, an AAO nano pattern with the interpore distance of 27 nm and the pore diameter of 7 nm was obtained. This is the smallest pattern, as long as we know, reported till now with AAO technique. The fabricated AAO pattern could be utilized for uniform and high density quantum dots with increased quantum effect.     

Electrochemical characteristics of surface of titanium formed by electrolytic polishing and anodizing

A clear surface was polished using electrolytic polishing (EP). The mean roughness (Rz) of the polished surface was 1.966 nm, as measured by atomic force microscopy (AFM) over a 2 × 2 um² scan area. The various directions of the grains could be observed clearly following EP. The multiple beam interference effect generated various colors of the grains after anodic treatment at constant anodic voltage. A template with ordered nanochannel-array of anodic titanium oxide (ATO) was formed at 20 V. The template formed by self-assembly. The long-range ordered nanochannel had a thickness of 170 nm film, a pore size of 100 nm, an inter-pore distance of 120 nm, pore walls with a thickness of 25 nm, a pore density of 8× 10⁹ pores/cm², and a porosity of 68.2%, after anodizing for 90 s. When the applied voltage exceeded the breakdown voltage (90 V) of titania, the corrosion rate increased and the color of the titanium became as measured electrochemically by Tafel polarization and AC impedance methods, and observed by optical microscopy.     

阳极氧化铝作为铝电解电容器阳极箔用的研究

采用直流电阳极氧化法在高纯铝箔上制备了多孔阳极氧化铝(AAO)膜,同时采用扫描电子显微镜(SEM)、循环伏安(CV)和电化学阻杭谱(EIS)等技术对AAO膜的表面形貌、厚度和比表面电容性质等进行了表征.结果表明,AAO膜由垂直于膜表面的、孔径在60～80nm之间的平行纳米孔道组成,膜的多孔层厚度约为20μm左右;AAO...     

Fabrication of highly ordered anodic aluminium oxide templates on silicon substrates

The controlled fabrication of highly ordered anodic aluminium oxide (AAO) templates of unprecedented pore uniformity directly on Si, enabled by new advances on two fronts - direct and timed anodisation of a high-purity Al film of unprecedented thickness (50 mum) on Si, and anodising a thin but pre-textured Al film on Si, has been reported. To deposit high-quality and ultra-thick Al on a non-compliant substrate, a prerequisite for obtaining highly ordered pore arrays on Si by self-organisation while retaining a good adhesion, a specially designed process of e-beam evaporation followed by in situ annealing has been deployed. To obtain an AAO template with the same high degree of ordering and uniformity but from a thin Al film, which is not achievable by the self-organisation alone, pre-patterning of the thin Al surface by reactive ion etching using a freestanding AAO mask that was formed in a separate process was performed. The resultant AAO/Si template provides a good platform for integrated growth of nanotube, nanowire or nanodot arrays on Si. Template-assisted growth of carbon nanotubes (CNTs) directly on Si was demonstrated via a chemical vapour deposition method. By controllably removing the AAO barrier layer at the bottom of the pores and partially etching back the AAO top surface, new CNT/Si structures were obtained with potential applications in field emitters, sensors, oscillators and photodetectors.     

Effect of pulse voltage and aluminum purity on the characteristics of anodic aluminum oxide using hybrid pulse anodization at room temperature

Most of the anodic aluminum oxide (AAO) templates are performed by potentiostatical method at 0-10 °C to inhibit the Joule's heat enhanced dissolution in aluminum oxide for well-ordered cell configuration. In this article, we propose the hybrid pulse anodization (HPA) method with effective suppression of Joule's heat generation to fabricate AAO at room temperature. Effects of purity of aluminum (Al) foils and pulse voltage on the evolution of pore characteristics have been investigated. The AAO morphology is captured by scanning electron microscope and analyzed via gray-scale imaging in order to identify the pore size distribution. The increased applied potential results in the widened pores and non-uniform cell arrangement due to the increased current density and variation. Moreover, low-purity Al foils lead to the reduced AAO distribution uniformity owing to the uneven electric field induced pits on the Al surface for inferior pore arrangement. Extending both the positive and negative pulse period from 1 s to 5 s during HPA can enhance the distribution uniformity of AAO from high-purity Al by up to about 95%. In addition, the relationship between AAO configuration and Al purity and pulse voltage is further discussed and established.