电子束蒸发法在多孔氧化铝膜上制备银纳米点阵列

采用二步阳极氧化法在草酸溶液中制备了高度有序的多孔阳极氧化铝(Porous Anodic Alumina,PAA)薄膜。以多孔氧化铝薄膜为模板,采用真空电子束蒸发的方法在多孔氧化铝模板上制备出了高度有序的金属银纳米点阵列体系。扫描电镜(SEM)测试结果表明,所制备的金属银纳米点阵列与多孔阳极氧化铝膜的多孔阵列具有完全相同的有序结构,阵列中银纳米颗粒的形状接近球形,其直径大约为70nm,与氧化铝模板的孔径基本一致。研究了高度有序银纳米点阵列的形成过程。     

多孔氧化铝膜上自组织生长Sn纳米点阵列的研究

以多孔阳极氧化铝膜(porous anodic alumina, PAA)为基片，采用真空电子束蒸发的方法在多孔氧化铝膜上制备了高度有序度的Sn纳米点阵列.锡纳米点阵的XRD与块体锡的完全相同，扫描电镜(SEM)测试结果表明，所制备的金属Sn纳米点阵与阳极氧化铝膜的多孔阵列具有完全相同的有序结构，阵列中每个Sn纳米粒子的形状为球形的，其直径接近于PAA膜的孔直径.对Sn纳米点阵形成过程和形成机理进行了讨论.     

Investigation of the super-long alumina nanowire array synthesized with a novel method

Alumina nanowire array standing on porous anodic alumina (PAA) membrane has been directly and efficiently synthesized in oxalic acid solution by one-step electrochemical anodic oxidation with changing anodic voltages. The morphology of the nanowires on PAA was observed by scanning electron microscopy (SEM). The different patterns on the surface of the sample were synthesized due to the reaction time. The fine structure of the patterns has shown that the pattern is composed of the alumina nanowire array and the morphologies of the patterns can mainly be attributed to the differences in the length of the alumina nanowires. The method of selected area electron diffraction (SAED) for transmission electron microscopy (TEM) has shown that these nanowires are amorphous. An etching model was given to explain the formation mechanism of the amorphous alumina nanowires.     

含分枝铜纳米线多孔铝膜的偏振特性

利用二次阳极氧化法制备了具有分枝结构的多孔铝(PAA)模板,并以交流电化学沉积的方法在该模板中合成了分枝状的铜纳米线。用SEM观察样品的形貌结构,用分光光度计测量了样品的透射光谱和偏振光谱。实验结果表明,含分枝状铜纳米线结构的多孔铝膜在近红外光区具有较高的透射率,且得到了14～22 dB的消光比。这种微偏振器件制备方法简单、效率高、造价低,在光电集成领域有着广泛的应用前景。     

A new routine to fabricate Bi single crystalline tapering junction nanowire arrays

Large-scale tapering junction Bi nanowire arrays have been synthesized by pulsed electrodeposition within a porous anodic alumina membrane (AAM). Bi metal–semiconductor and semiconductor–semiconductor junction nanowires with different diameters were fabricated easily by modulating only the pulse time using only an ordinary AAM template. The morphology and structure of the tapering junction Bi nanowire arrays and individual nanowires are characterized by scanning electron microscopy and transmission electron microscopy. The voltage–current measurements show the intrinsic nonlinear and asymmetric characteristics of metal–semiconductor junction nanowires. PACS 81.05.Bx; 82.80.Fk; 73.63.Nm     

利用扫描电镜和原子力显微镜测量纳米微孔阳极氧化铝膜

利用多孔型阳极氧化铝膜（PAA）制备纳米材料是近年来研究的热点之,对PAA的形貌进行准确的表征具有重要的意义,文章首先分析了传统扫描电镜（SEM）观测方法中镀膜工艺对样品和测量结果的影响,并提出了对镀膜过渡区进行观测的方案,然后着重研究了利用原子力显微镜（AFM）对PAA进行无损测量的方法,比较了不同测量模式下的测量结果,并利用Reiss模型对“针尖-样品卷积效应”进行了有效的修正,文章的研究结果不仅适用于多孔型阳极氧化铝膜这一研究领域,对于纳米多孔材料的测量也有普遍的参考价值。     

基于包络线法的多孔阳极氧化铝薄膜光学常数的计算

采用二步阳极氧化法在草酸溶液中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。结果发现,在其表面孔径为30~40nm的六边形孔洞分布均匀,且垂直于表面平行生长。依据PAA透射光谱的实验数据,采用极值包络线算法计算出了PAA薄膜的复折射率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发现,PAA薄膜具有直接带隙半导体的电子结构特征,而且由理论计算得到的PAA的带隙能与其光致发光谱的峰位能是一致的。     

Selective tungsten deposition into ordered nanohole arrays of anodic porous alumina by electron-beam-induced deposition

The selective deposition of a metal (tungsten) into ordered nanohole arrays of an anodic porous alumina membrane was performed using an electron-beam-induced deposition process. After deposition, the membrane was observed and analyzed using electron microscopy and energy-dispersive X-ray spectroscopy. It is shown that the deposition was preferentially conducted in the holes in the irradiated area of the electron beam. A calculation of the electron-beam intensity explains the reason for the preferential deposition in the holes. PACS 81.07.-b; 81.16.Rf; 61.46.+w     

Electrochemical synthesis of ordered CdTe nanowire arrays

Semiconductor CdTe nanowire arrays embedded in the nanochannels of the porous anodic alumina (PAA) template have been prepared by using a potentiostatic electrochemical deposition method. The morphology and structure of the CdTe nanowire arrays have been characterized by X-ray powder diffraction, transmission electron microscopy, and high-resolution transmission electron microscopy. It is found that the CdTe nanowires with diameters and lengths of about 60 nm are single-crystalline with cubic phase structure, uniformly and continuously embedded in the nanochannels of the PAA template. X-ray energy-dispersion analysis and X-ray photoelectron spectroscopy analysis indicate that stoichiometric CdTe was formed. The growth mechanism of the CdTe nanowires is also discussed. Received: 11 June 2002 / Accepted: 2 July 2002 / Published online: 8 January 2003 RID="*" ID="*"Corresponding author. Fax: +86-551/559-1434, E-mail: aiwuzhao@yahoo.com.cn     

Fabrication of well-aligned CdS nanotubes by CVD-template method

Well-aligned CdS nanotubes have been synthesized within the nanochannels of the porous anodic alumina (PAA) membranes by pyrolyzing cadmium bis(diethyldithiocarbamate) [Cd(S₂CNEt₂)₂] at 400 °C. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) show that the CdS nanotubes are highly ordered with uniform diameter in range of 80-150 nm and the length up to tens of microns. X-ray diffraction (XRD), Raman spectrum, energy-dispersive spectroscopy (EDS) and selected-area electron diffraction (SAED) demonstrate that the nanotubes are composed of pure hexagonal phase polycrystalline CdS. The synthetic route can, in principle, be extended to fabricate other nanotubes of a wide range of semiconductors.     

Si nanopillar arrays with nanocrystals produced by template-induced growth at room temperature

Well-aligned and closely-packed silicon nanopillar (SNP) arrays are fabricated by using a simple method with magnetron sputtering of Si on a porous anodic alumina (PAA) template at room temperature. The SNPs are formed by selective growth on the top of the PAA pore walls. The growth mechanism analysis indicates that the structure of the SNPs can be modulated by the pore spacing of the PAA and the sputtering process and is independent of the wall width of the PAA. Moreover, nanocrystals are identified by using transmission electron microscopy in the as-deposited SNP samples, which are related to the heat isolation structure of the SNPs. The Raman focus depth profile reveals a high crystallization ratio on the surface.     

Synthesis and magnetic properties of multilayer Ni/Cu and NiFe/Cu nanowires

Highly ordered composite nanowires with multilayer Ni/Cu and NiFe/Cu have been fabricated by pulsed electrodeposition into nanoporous alumina membrane. The diameter of wires can be easily varied by pore size of alumina, ranging from 30 to 100 nm. The applied potential and the duration of each potential square pulse determine the thickness of the metal layers. The nanowires have been characterized by transmission electron microscopy (TEM), magnetic force microscopy (MFM), and vibrating sample magnetometer (VSM) measurements. The MFM images indicate that every ferromagnetic layer separated by Cu layer was present as single isolated domain-like magnet. This technique has potential use in the measurement and application of magnetic nanodevices.     

Polarization properties of porous anodic alumina with Y-branched Cu nanowires

Porous anodic alumina (PAA) templates with branch structure are fabricated by the two-step anodic oxidation processes, and then the Y-branched Cu nanowires are synthesized in the templates using an alternating current (AC) deposition method. We observe the morphology image of the samples by scanning electron microscopy (SEM), and measure the transmission spectrum and the polarization spectrum of the samples by the spectrophotometer. The results show that PAA films with Y-branched Cu nanowires have better transmittance in the near infrared region. An extinction ratio of 15-18 dB and an insertion loss of 0.1-0.4 dB are obtained in this region. Therefore PAA with Y-branched Cu nanowires can be used as a near-infrared micropolarizer, and this kind of micropolarizer would have a promising future in the field of photoelectricity integration.     

强辐射源用铜纳米线阵列靶的结构与性能

 采用多孔阳极氧化铝（AAO）模板脉冲电沉积法制备了强辐射源用铜纳米线阵列靶,并用扫描电子显微镜（SEM）、能谱（EDS）和X射线衍射（XRD）对其进行了结构表征。结果表明：去除AAO模板后铜纳米线平均直径比去除AAO模板前的平均孔径大32%,长度缩短5%。对电沉积2 000 s的样品进行铜纳米线长度分布表征,结果显示:距离模板圆心越远,铜纳米线越长。与超短脉冲激光相互作用实验结果表明:纳米线平均长度在18~50 μm范围内,铜Kα光子产额先随纳米线长度增加而增加,当长度大于33 μm时,铜Kα光子产额开始下降。     

银纳米有序阵列SERS活性基底的制备及在膀胱肿瘤细胞检测中的应用

以多孔阳极氧化铝(porous anodic alumina,PAA)膜为模板,采用真空电子束蒸镀技术,分别在PAA多孔层以及阻挡层表面形成了银纳米孔和银纳米帽有序阵列表面增强拉曼散射(surface-enhancedRaman scattering,SERS)活性基底,并以膀胱肿瘤细胞作为分子探针,测试和分析了这两种SERS活性基底的表面增强拉曼光谱的特性。结果表明,两种SERS活性基底对膀胱肿瘤细胞的拉曼散射信号均有很好的增强作用。银纳米帽有序阵列SERS活性基底不仅具有较高的SERS增强和荧光猝灭效应,而且不存在与PAA膜中草酸根杂质相关的干扰峰,可获得膀胱肿瘤细胞拉曼散射光谱的更多细节信息。     

Diameter-dependent electrical transport properties of bismuth nanowire arrays

Single-crystalline bismuth nanowire arrays with different diameters were fabricated within porous anodic alumina membranes with the same pore size using the pulsed electro-deposition technique. X-ray diffraction measurements show that the as-synthesized nanowires have a highly preferential orientation. Scanning electron microscopy, transmission electron microscopy and high-resolution transmission electron microscopy analyses indicate that bismuth nanowire arrays are high filling, ordered and single-crystalline. Electrical resistance measurements show that the bismuth nanowires have a metal-semiconductor transition when the diameters decrease from 90 to 50 nm, and the resistance behaviors are explained on the basis of the quantum confinement effect and Matthiessen’s rule.     

Morphology and transmittance of porous alumina on glass substrate

The porous optical film has higher threshold of laser-induced damage than densified films, for the study of mechanism of laser-induced damage of porous optical film with ordered pore structure. Porous anodic alumina (PAA) film with high transmittance on glass substrate has been prepared. Aluminum film was deposited on glass substrate by means of resistance and electron beam heat (EBH) evaporation. Porous alumina was prepared in oxalic acid solution under different anodizing conditions. At normal incidence, the optical transmittance spectrum over 300-1000 nm spectra region was obtained by spectrophotometer. SEM was introduced to analysis the morphology of the porous alumina film. The pore aperture increased with the increase of anodizing voltage, which resulted in a rapid decrease of the pore concentration and the optical thickness of porous alumina film. Damage morphology of porous alumina film is found to be typically defects initiated, and the defect is the pore presented on the film.     

Electrochemical fabrication and characterization of lepidocrocite (γ-FeOOH) nanowire arrays

We report on the fabrication of γ-phase iron oxyhydroxide (γ-FeOOH, lepidocrocite) nanowire (nw) arrays within the alumina pores by electrodeposition. An aqueous solution, friendly to alumina matrix, was generated and applied in this study for uniform deposition of γ-FeOOH nw arrays directly through the alumina barrier layer using an alternating current (ac) mode. As-deposited nanowired products were characterized using ⁵⁷Fe Mössbauer spectroscopy (MS), atomic absorption spectrophotometry analysis, field-emission scanning electron microscopy, UV-vis transmission spectroscopy, transmission electron microscopy and X-ray diffraction. The formation of pure lepidocrocite nw arrays in the alumina pores with the average Ø_pore of 45 and 150 nm was verified by transmission MS at cryogenic temperatures.     

Study the effect of striping in two-step anodizing process on pore arrangement of nano-porous alumina

Two-step anodic oxidation of aluminum is generally employed to produce the ordered porous anodized alumina (PAA). Dissolving away (striping) the oxide film after the first anodizing step plays a key role in the final arrangement of nano-pores. In this work, different striping durations between 1 and 6 h were applied to the sample that was initially anodized at a constant voltage of 40 V at 17 °C for 15 h. The striping duration of 3 h was realized as the optimum time for achieving the best ordering degree for the pores. Scanning electron microscopy (SEM) was used during and at the end of the process to examine the cross section and finishing surface of the specimens. Linear-angular fast Fourier transform (LA-FFT), an in-house technique based on MATLAB software, was employed to assess the ordering degree of the anodized samples.     

Fabrication of metal nano-structures using anodic alumina membranes grown in phosphoric acid solution: Tailoring template morphology

The influence of experimental parameters on the morphology of the porous structure and on the formation kinetics has been investigated for anodic alumina membranes (AAM) grown in aqueous H₃PO₄ at 160 V. It was found that pore aspect ratio and membrane porosity on the solution-side surface are influenced by tensiostatic charge, bath temperature and the presence of Al³⁺ ions in solution. Morphological and kinetic data, recorded in different conditions, give useful information on the growth mechanism of pore channels in phosphoric acid solution.Nickel nano-structures have been fabricated using AAM as template. Electroless deposition, performed by adding the reducing agent to a suitable bath in several steps, resulted in the formation of short metal nanotubes (about 5 μm long) in the upper part of the channels. Long Ni nanowires (up to 25 μm) with aspect ratio higher than 100 were obtained by pulsed unipolar electrodeposition from a Watt bath. In this case, both the influence of some experimental parameters on the nanowires growth and the fast current transients during the electrodeposition steps were analyzed.