草酸阳极氧化工艺对氧化铝模板孔径的影响

为了寻找出草酸氧化工艺和扩孔工艺对制备的氧化铝模板孔径大小的影响规律,本文采用高倍扫描电镜观察定量研究了纯铝草酸阳极氧化几种氧化工艺参数对制备的氧化铝模板纳米孔径大小的影响,并对氧化铝模板的扩孔工艺进行了研究.结果表明,随着草酸浓度、氧化电压、氧化温度的升高和氧化时间的延长,制备的氧化铝模板的孔径也随着增加;在扩孔溶液浓度、温度保持一定时,随着浸泡时间的延长,氧化铝模板的孔径会逐渐增大.本研究结果为模板合成有序纳米阵列结构提供了参考.     

阳极氧化法制备有序纳米多孔氧化铝膜的研究

利用电化学阳极氧化的方法,在草酸溶液中,精确控制反应条件,在高纯铝片表面有序生长了纳米多孔氧化铝膜。试验中,分别采用一次阳极氧化和二次阳极氧化方法制备氧化铝膜。利用H3PO4溶液浸泡法对氧化铝膜进行扩孔处理。通过扫描电子显微镜对样品进行表征分析。结果发现,二次阳极氧化制备的氧化铝膜的孔洞分布较一次氧化的更为规则有序,并且孔径大小均匀一致。扫描电镜观察显示,氧化铝膜的扩孔过程可以去掉阻碍层,并调节孔径大小,溶去二次氧化后黏附在氧化层表面的一些杂质,从而使氧化铝模板更为规则有序,孔径均一。这种经过二次阳极氧化和扩孔处理得到多孔阳极氧化铝模板的方法简单,成本较低,可以为后续的纳米材料合成提供高质量的合成模板。     

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.     

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。     

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.     

多孔阳极氧化铝模板上电子束蒸发沉积TiO_2

以硫酸、草酸溶液为电解液,采用二次阳极氧化法制备了初始孔径在20~120 nm、孔间距在40~250 nm、孔深在200 nm~80μm范围内的具有高度有序纳米孔阵列的多孔阳极氧化铝(porous anodic alumina,PAA)模板。以PAA模板为基片,采用真空电子束蒸发的方法在PAA模板上制备了具有高度有序的TiO2纳米点阵列。利用场发射扫描电子显微镜和原子力显微镜对其形貌进行了表征。研究表明,所形成的TiO2纳米点阵列具有同其基底PAA模板相同的序列结构。对TiO2纳米点阵列的生长形成机理进行了讨论。     

外表面不同孔结构的阳极氧化铝模板的自组织制备

经二次阳极氧化制备了外表面不同孔结构的阳极氧化铝模板.用场发射扫描电镜(FE-SEM)对其形貌进行表征,发现在直接阳极氧化的铝箔的外表面自组装形成了规则的六方形的纳米孔,而在去除铝基、扩孔的另一外表面则形成了规则的圆形的纳米孔,外表面纳米孔的平均直径大约为80nm,孔间距大约为110nm,孔密度约为2.5×10n cm-2.在模板的内部形成相互平行且垂直于AAO模板外表面的纳米管的阵列结构,纳米管的平均直径大约为80nm;AAO模板的厚度大约为10/zm.粉末X射线衍射(XRD)表明模板具有非晶态的结构.记录了阳极氧化过程中的电流一时间曲线,探讨了自组织孔洞的形成机理,提出了新型阳极氧化铝模板制备纳/微米结构材料模拟应用.     

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.     

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.     

单通氧化铝模板的制备及工艺优化

利用高纯铝片采用两步阳极氧化法制得排列高度有序、尺寸可控的单通氧化铝(anodic aluminum oxide templates,AAO)模板,且纳米孔呈六方形结构。分别探究了预处理条件、氧化次数、扩孔时间等对AAO模板尺寸及有序性的影响。结果表明,预处理利于纳米管形成高度有序结构,并发现二次阳极氧化法比一次阳极氧化法制备的纳米管排列更有序且孔径均匀;在0~75 min内,管孔径与扩孔时间呈线性关系,酸溶液对孔的腐蚀速率为0.601nm/min,在0~120min内,管长度与二次氧化时间呈线性关系,生长速率为0.28μm/min;最佳电解液浓度确定为0.3mol/L。为后续制备非对称丝岛状骨组织再生高分子薄膜奠定了良好基础。     

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.     

Large-scale patterning of gold nanopillars in a porous anodic alumina template by replicating gold structures on a titanium barrier

Gold nanopillars are grown in patterns inside a porous anodic alumina template. On selected positions, defined by a gold "seed" pattern, gold is electroplated into the pores, while a barrier layer underneath the porous template blocks the deposition on the rest of the surface. Large-scale arrays of free-standing nanopillar islands are obtained after selective etching of the alumina template.     

高度有序多孔氧化铝模板的制备工艺与生长机制的研究

采用二次氧化法制备出高度有序的多孔氧化铝模板，结合扫描电镜和原子力显微镜对其结构、形貌进行观察和表征。研究了铝箔预处理和温度等对多孔氧化铝模板孔洞有序性的影响，讨论了有序孔洞的自组织生长机理。     

Synthesis of porous oxide ceramics using a soft responsive scaffold

Ceramic materials have significant utility. Developing synthetic protocols that are facile and provide low energy alternatives to traditional methods remains a major driver in materials synthesis. We present here the adaptation of a method recently developed in our group for the synthesis of porous silica using a non-ionic emulsion template. The silicate materials are porous on both the nanometre and micrometre length scales and surface-to-volume ratios may be readily modified by altering the volume fraction of the emulsion template. Switching the silica precursor for an alumina or titania precursor resulted in the formation of porous alumina and titania materials which were prepared as thin films or monoliths. The pores formed in the amorphous alumina materials were ~0.8 μm and ~50 nm, with a primary particle size of 50–100 nm. The titania materials had pores on one length scale only: ~0.8 μm, with a smaller primary particle size of 20–60 nm. As-synthesized materials were investigated using scanning electron microscopy and X-ray diffraction.     

Sputter deposition of self-organized nanoclusters through porous anodic alumina templates

Silver nanoparticles were sputter deposited through self organized hexagonally ordered porous anodic alumina templates that were fabricated using a two-step anodization process. The average pore diameter of the template was 90 nm and the interpore spacing was 120 nm. Atomic force microscope studies of the sputter-deposited silver nanoparticle array on a Si substrate indicate an approximate replication of the porous anodic alumina mask. The nature of the deposition depends strongly on the process parameters such as sputtering voltage, ambient pressure and substrate temperature. We report a detailed study of the sputtering conditions that lead to an optimal deposition through the template.     

用AAO模板法制备硅纳米管

先用二步阳极氧化法制备纳米孔平均孔径约为100 nm的Al/Al_2O_3(AAO)模板,再以AAO为模板用溶胶-凝胶法合成管径约为60-80 nm的硅纳米管,并用扫描电镜和透射电镜观察了硅纳米管的形貌。结果表明,AAO模板的孔径分别随着二步阳极氧化法中电解温度、氧化电压、硫酸和草酸混酸浓度的增大而增大,硅纳米管的形成与硅烷溶胶的嵌入方法、凝胶形成时间和温度有较大的关系。     

Fabrication of mesoporous titanium oxide nanotubes based on layer-by-layer assembly

Titanium oxide (TiO2)/polyacrylic acid (PAA) composite nanotubes were firstly fabricated through the sol-gel process of titanium alkoxide in the inner pores of alumina template followed layer-by-layer assembly with polyacrylic acid (PAA). Mesoporous TiO2 nanotubes could be obtained after the removal of PAA component by calcination and etching of the template with concentrated sodium hydroxide aqueous solution. The surface area of as-prepared porous TiO2 nanotubes was measured as twice larger than that of the conventional TiO2 nanotubes and the pore diameter in the wall of the tubes is several nanometers. Such assembled mesoporous nanotubes can serve as carriers for catalysis release and biomolecules.     

以修饰的PAA模板制备Ni纳米线的研究

采用直流电沉积法制备了Ni纳米线,用SEM和TEM测试手段观察产物形貌,结果表明,合成的纳米线阵列具有排列有序、彼此平行等特点,XRD、EDX、SQUID测试手段研究了产物化学成份和磁学性质,实验发现,Ni纳米线的矫顽力在退火前后分别为67 Oe和774 Oe。     

Electrodeposited bismuth telluride nanowire arrays with uniform growth fronts

Bismuth telluride (Bi2Te3) nanowires were deposited into porous alumina templates with 35 nm diameter pores by a pulsed-potential electrodeposition method. For growth at temperatures between 1 and 4 degrees C, the nanowires filled 93% of the pores of the template, and the growth fronts were uniform with nanowire lengths of approximately 62-68 microm. There are over ten billion nanowires per square centimeter with aspect ratios approaching 2000:1. Samples were characterized by scanning and transmission electron microscopy, X-ray diffraction, and electron microprobe analysis. The crystalline nanowire arrays are highly oriented in the [110] direction, which is optimal for thermoelectric applications.