One-step anodization fabrication and morphology characterization of porous AAO with ideal nanopore arrays

A fabrication method for one-step anodization of an anodic aluminum oxide (AAO) template with nanopore arrays using pretreated high purity aluminum foil is reported in this article. Morphology of the AAO was characterized by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Results showed that porous AAO with ideal nanopore arrays can be fabricated by one-step anodization fabrication technology on high purity aluminum foil which had been anodized at 45?V direct current (DC), in 0°C, 0.5?M H₂C₂O₄ solution for 48 hours. The average pore diameter and the interpore distance were 80?nm and 120?nm, respectively. Nanopores in porous AAO had very narrow size distribution and were arranged into hexagonal array. The formation mechanism of nanopore arrays in porous AAO is discussed. Porous AAO with ideal nanopore arrays provide an ideal template for preparation of many one-dimensional nanomaterials. One-step anodization of AAO is a simpler procedure and more applicable in industrial application than the previous two-step anodization technology.     

Niobium and hafnium grown on porous membranes

In this work we report on a method for fabricating highly ordered nanostructures of niobium and hafnium metals by physical vapour deposition using two different templates: anodized aluminum oxide membranes (AAO) and zirconium onto AAO membranes (Zr/AAO). The growth mechanism of these metal nanostructures is clearly different depending on the material used as a template. A different morphology was obtained by using AAO or Zr/AAO templates: when the metal is deposited onto AAO membranes, nanospheres with ordered hexagonal regularity are obtained; however, when the metal is deposited onto a Zr/AAO template, highly ordered nanocones are formed. The experimental approach described in this work is simple and suitable for synthesizing nanospheres or nanoholes of niobium and hafnium metals in a highly ordered structure.     

A kind of synthetic nanopillar arrays for studying single biomolecule

The anodic aluminum oxide (AAO) template with ordered pores was firstly fabricated in oxalic acid solutions using two-step anodization method. Then, a layer of polymethylmethacrylate (PMMA) was uniformly laid on one surface of the AAO template by a Spin-Coater, then baked and cooled them, after that, the H3PO4 solution was utilized to dissolve the residual aluminum and barrier layer, as the result, the functional nanopillar arrays were achieved. Finally, the morphology of the functional PMMA nanopillars was examined with the Scanning Electron Microscope (SEM) and the properties were discussed. The functional nanopillar arrays could be applied to the micro and nano-scale devices as the sensors for the biological, chemical and single molecular detection.     

导电聚合物纳米线的制备及气敏性能研究

首次采用简单的浸润多孔氧化铝(AAO)模板法制备了导电聚合物聚-3,4-乙烯二氧噻吩(PE-DOT)纳米线.导电聚合物溶液浸润AAO模板后,PEDOT吸附于孔道壁并进一步聚合生成导电聚合物纳米线.紫外-可见光-近红外光谱(UV-vis-NIR spec-trum)分析表明生成的纳米线处于掺杂态.采用四探针仪分析了导电聚合物纳米线的导电性能,结果显示纳米线电导率相比普通PEDOT材料有数量级增加,且表现出良好的掺杂/脱掺杂能力.研究了导电聚合物纳米线的气体敏感性能,发现其对挥发性醇类,尤其对甲醇在较低浓度下表现出优异的敏感性,对5×10-6甲醇气体的响应时间约为10～20s,测试可重复性超过20次,达到饱和吸附时的气体浓度明显大于普通PEDOT材料.表明PEDOT纳米线不仅提供了较大表面积供气体分子吸附,而且纳米线中导电通道取向一致,从而体现出较好的气体敏感性能.     

用低纯度铝制备AAO模板及其结构研究

在0.3mol/dm3草酸溶液中,通过不同纯度铝的恒电位二次阳极氧化制备了纳米孔氧化铝模板,并用场发射扫描电子显微镜(FE-SEM)和原子力显微镜(AFM)观察模板结构.实验结果表明,一次氧化除膜后低纯度铝基体表面呈现较为规则的六边形结构,这种蜂巢结构有利于二次氧化过程中获得有序度更高的纳米孔模板.低纯度铝制备的模板表面被晶界分隔为微小的区域,只是在较窄区域内才出现六边形规则排列的纳米孔.恒电位40V时所得模板经扩孔处理后,孔径由35nm增大到100nm左右,且孔径大小几乎一致.从纳米孔的有序度来看,由低纯度铝制备模板还需要进一步优化阳极氧化参数.     

聚合物分子量对浸没沉淀法制备PVDF微孔膜结构与结晶的影响

聚合物的分子量对浸没沉淀法制备聚偏氟乙烯(PVDF)微孔膜结构和结晶具有较大影响。随着聚合物分子量的增大,所成膜上表面孔尺寸和孔密度有减小的趋势。分子量较大的PVDF所成膜的底面及膜内指状孔表面均为完全无孔致密结构。断面指状孔下方为相互连通的海绵状结构。当聚合物的分子量较低时,断面开始由相互连通的海绵状结构向胞腔状结构过渡。由低分子量的PVDF制得的膜,结晶类型既有α型结晶,又有β型结晶。由高分子量的PVDF制得的膜,主要为α型PVDF结晶。后者的结晶度明显大于前者。     

Scaling down lateral dimensions of silicon nanopillars fabricated by reactive ion etching with Au/Cr self-assembled clusters as an etch mask

Nanodot and nanopillar structures and precisely controlled reproducible fabrication thereof are of great interest in common nanoelectronic devices, including photonic crystals and surface plasmon resonance instruments. In this work, fabrication process of the silicon nanopillar structures is described. It includes self-organization of gold and chromium clusters at thickness close to that of one atomic diameter to serve as etching masks followed by the reactive ion etching to form silicon nanopillars. Scanning electron microscopy and X-ray photoelectron spectroscopy were used to characterize self-organized gold and chromium clusters as well as the final silicon nanopillars. This method was found to produce silicon nanopillars of sub-10 nm lateral dimensions and the diameter-to-height aspect ratio of up to 1:14.     

Nanomechanical and surface behavior of polydimethylsiloxane-filled nanoporous anodic alumina

In this article, the mechanical and wetting behavior of anodic aluminum oxide (AAO) and nanoporous-filled AAO were investigated using nanoindentation and contact angle measurements. The results showed that the nanoporous AAO was hydrophobic with a contact angle of 105°. The polymer filling affected the surface property and reduced the contact angle to 84°. The effects of the nanoporous filling on the Young’s modulus and the hardness are investigated and discussed. A three-dimensional finite element model was also successfully developed to understand the nanoindentation-induced mechanism. A maximum von Mises stress of 1058 MPa occurred beneath the indenter.     

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.     

静电纺丝与静电喷雾技术共纺制备PPESK/PVDF复合锂电池隔膜

为了改善传统静电纺丝无纺布纤维膜力学性能较差的缺点,采用静电纺丝和静电喷雾技术相结合的方法,同时进行静电纺PPESK浓溶液和PVDF稀溶液,制备得到PPESK纤维/PVDF珠粒复合锂电池隔膜,并在160℃进行热压后处理。通过扫描电子显微镜、万能拉伸试验机、电化学工作站及充放电测试仪等表征复合锂电池隔膜的微观结构、力学性能、离子电导率和相应的电池充放电性能。结果表明,该复合隔膜具有良好的电解液润湿性,室温下离子电导率达到1.92mS·cm^-1,PVDF珠粒均匀地分布在PPESK纤维中,珠粒经热压产生微熔融有效增强了纤维之间的黏结力,使复合膜的力学强度提高到13.2MPa。此外,使用复合隔膜装配的电池展现出较高的放电比容量和稳定的循环性能。     

Investigation of sisal fibers by atomic force microscopy: morphological and adhesive characteristics

Atomic force microscopy (AFM) was used to study the nanoscale surface chemistry and morphological changes caused by chemical treatment of sisal fibers. Scanning Electron Microscopy (SEM) micrographs indicated that sisal in natura (bundle of fibers) is formed by fibers with diameters of approximately 10 microm. AFM images showed that these fibers consist of microfibrils with diameters varying from 250 to 600 nm, which are made up of nanofibrils of ca. 20 nm in diameter. The adhesion force (pull-off force) between the AFM tip and the fibers surface increased after benzylation, pointing to a decrease in the polar groups on the sisal fiber. The adhesion map measured over a scan range of 3 microm was heterogeneous in samples treated with 40% NaOH and the low adhesion sites disappeared after benzylation. Using an established mathematical model, it was possible to evaluate the increase in adhesion work and consequently in the interaction between the AFM tip and sisal fibers. These results indicated that AFM can detect heterogeneity in the wettability of sisal fibers with nanometer resolution and can be applied in the study of fiber-matrix adhesion in polymer composites.     

Electrospinning of aligned biodegradable polymer fibers and composite fibers for tissue engineering applications

Fibrous membranes of aligned poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV) fibers have been made through electrospinning. A high-speed rotating drum was used as the fiber collector while the electric field was manipulated by using five knife-edged auxiliary electrodes. It was found that a high drum rotating speed of 3000 rpm could lead to a nearly perfect alignment of PHBV fibers during electrospinning. Multilayered fibrous structures with each layer having a different direction of fiber alignment could also be constructed through electrospinning. The electrospun PHBV fibers were further modified by incorporating carbonated hydroxyapatite (HA) nanospheres (up to 20% of HA) in the fibers. The fibrous membranes made of aligned PHBV fibers and made of HA/PHBV composite fibers should be very useful for the tissue engineering of different human body tissues.     

热致相分离法制备聚偏氟乙烯微孔膜

对聚偏氟乙烯(PVDF)/碳酸二苯酯(DPC)体系,采用热致相分离(TIPS)法制备了PVDF微孔膜.通过稀释剂的溶度参数对体系的相容性进行分析,热力学相图和不同PVDF质量浓度下制备的微孔膜断面照片均证明该体系具有较宽的液-液相分离区.PVDF/DPC体系偏晶点对应的PVDF浓度约为质量分数56%,低于此浓度体系降温后先发生液-液相分离,随着PVDF浓度的增大,微孔膜断面结构由双连续结构转变为蜂窝状结构,且膜孔孔径减小,高于此浓度体系降温后只发生固-液相分离,微孔膜断面呈块状紧密堆积结构.较快的冷却速率有利于低PVDF浓度时较小孔径膜和高PVDF浓度时较小球粒尺寸膜的生成.     

Preparation of polyaniline nanotubes array based on anodic aluminum oxide template

In this article, the highly ordered polyaniline (PANI) nanotubes array was prepared by in situ polymerization using anodic aluminum oxide (AAO) as template. Polymerization of aniline was confined in the one-dimensional nanochannel of AAO template. The aniline was adsorbed and polymerized preferentially on the pore walls of template. The structure of PANI nanotubes array was characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), selected area electron diffraction (SAED) and dynamic force microscope (DFM). The results show that PANI nanotubes are synthesized successfully in the nanopores of template, the diameter and length of PANI nanotubes are closed to the pore diameter and thickness of AAO template, respectively, the arrangement of PANI nanotubes is very regular and uniform, the crystal form of PANI nanotubes is hexagonal, different from pseudo-orthorhombic crystal form of PANI bulk sample, and cell parameters a and b are 0.5008 nm. The change of crystal form is due to the confinement of AAO template, which makes the molecular chain of PANI arrange more ordered.     

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.     

Optimization of the Sol–Gel Chemical Route for Fabrication of Densely Packed NiFe2O4 Nanowires in the AAO Template

In this paper we investigate the thermal decomposition of the citrate-based precursors in order to make the chemical and physical properties appropriate for the fabrication of nickel ferrite nanowires (NWs) through the sol?Cgel chemical route. IR spectroscopy (FTIR) along with X-ray diffraction (XRD) has been performed to select the suitable chemical and physical conditions for the sol?Cgel process. The anodic aluminum oxide (AAO) method was used for the template to control the diameter and length of the aligned wires. The morphology of the samples was studied by field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) techniques. The magnetic measurements were also done by a vibrating sample magnetometer (VSM). The results showed that the NiFe₂O₄ NWs were parallel ordered in the AAO template and their mean diameter is 80?C100?nm with high aspect ratio of 600.     

聚偏氟乙烯电纺纤维膜的制备及其热释电性能研究

β晶相的聚偏氟乙烯(PVDF)由于具有强压电和热释电特性,被广泛应用在能量收集、红外探测等领域。采用静电纺丝技术制备PVDF纤维,通过SEM以及XRD表征,研究了溶剂组成、溶液浓度和纺丝液供给速度等纺丝参数对PVDF纤维膜形貌和β晶相含量的影响,制备出连续、均匀、直径约600nm的PVDF纤维。另外,测试了PVDF纤维膜对不同调制频率的3.4μm波长红外光的热释电响应特性。     

Effect of fiber orientation in gelled poly(vinylidene fluoride) electrospun membranes for Li-ion battery applications

Battery separators based on electrospun membranes of poly(vinylidene fluoride) (PVDF) have been prepared in order to study the effect of fiber alignment on the performance and characteristics of the membrane. The prepared membranes show an average fiber diameter of ~272 nm and a degree of porosity of ~87 %. The gel polymer electrolytes are prepared by soaking the membranes in the electrolyte solution. The alignment of the fibers improves the mechanical properties for the electrospun membranes. Further, the microstructure of the membrane also plays an important role in the ionic conductivity, being higher for the random electrospun membrane due to the lower tortuosity value. Independently of the microstructure, both membranes show good electrochemical stability up to 5.0 V versus Li/Li⁺. These results show that electrospun membranes based on PVDF are appropriate for battery separators in lithium-ion battery applications, the random membranes showing a better overall performance.     

One-dimensional multiferroic bismuth ferrite fibers obtained by electrospinning techniques

We report the fabrication of novel multiferroic nanostructured bismuth ferrite (BiFeO(3)) fibers using the sol-gel based electrospinning technique. Phase pure BiFeO(3) fibers were prepared by thermally annealing the electrospun BiFeO(3)/polyvinylpyrrolidone composite fibers in air for 1 h at 600?°C. The x-ray diffraction pattern of the fibers (BiFeO(3)) obtained showed that their crystalline structures were rhombohedral perovskite structures. Both scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images revealed that the BiFeO(3) fibers were composed of fine grained microstructures. The grains were self-assembled and self-organized to yield dense and continuous fibrous structures. The magnetic hysteresis loops of these nanostructured fibers displayed the expected ferromagnetic behavior, whereby a coercivity of ～ 250 Oe and a saturation magnetization of ～ 1.34 emu g(-1) were obtained. The ferroelectricity and ferroelectric domain structures of the fibers were confirmed using piezoresponse force microscopy (PFM). The piezoelectric hysteresis loops and polar domain switching behavior of the fibers were examined. Such multiferroic fibers are significant for electroactive applications and nano-scale devices.     

The growth of ordered ZnAl2O4 nanostructures using AAO as a reactive template

The use of anodic aluminum oxide (AAO) as a reactive template in the fabrication of ordered arrays of spinel ZnAl₂O₄ nanostructures is demonstrated. This involves the growth of monocrystalline Zn nanowires into an AAO template using a pulse dc electrodeposition technique followed by a heat treatment in air at 800 °C. The formation of ZnAl₂O₄ nanotubes in the solid-state reaction is driven by the Kirkendall effect. In addition, the formation of such ZnAl₂O₄ nanostructure arrays requires that the molar ratio of ZnO to Al₂O₃ be less than unity. This corresponds to a ratio of pore radius to half inter-pore separation of 0.63 which serves as a guide to the initial template geometry required for the formation of an array of discrete nanotubes.