铂微电极位点上氧化铝纳米孔的制备

金属微电极表面的纳米级处理可以大大提高电极的性能。本文基于微加工及电化学技术在铂微电极位点上制备了一致性良好的氧化铝纳米结构。通过对基片铂层表面等离子体处理,使铝膜与铂层之间粘附力明显增强。利用二次阳极氧化法,在铂微电极位点上制备出纳米孔。结果表明,30V是该条件下比较理想的氧化电压。同时,通过对氧化过程中电流的监测,发现当铝膜完全氧化后电流大幅上升,可将此现象作为终止阳极氧化的标志。这种微电极位点处的氧化铝模板可进一步用于不同材料纳米微电极的制备。     

电化学制备P型硅基二维光子晶体优化参数

利用光刻技术与碱性腐蚀等工艺预写晶格图样,采用电化学腐蚀方法在P〈100〉型硅基底制备二维大孔硅光子禁带结构.结果表明:在预写有晶格图样的P〈100〉型硅基底上由电化学阳极氧化制备的二维大孔硅,其孔洞的生长速率、深宽比及表/侧面形貌与电解质配比方案及阳极电流密度均密切相关.在优化的电化学工艺参数下得到的空气洞阵列,具有近乎完美的二维四方晶格,晶格常数为3.8μm,孔洞直径约3.0μm,孔洞深宽约90μm,深宽比达30.该方法可用于制备在中红外或近红外波段具有完全二维光子带隙的光子晶体.     

多孔氧化铝有序膜的制备研究

本文用阳极氧化法分别在硫酸和草酸电解液中成功制备出高度有序、具有纳米级孔洞的氧化铝有序阵列模板。采用饱和HgCl₂去除Al基体后,得到典型六方形结构的多孔Al₂O₃有序膜。通过改变氧化电压、氧化时间等条件使模板的孔径、孔深可调、膜厚度可控,并系统研究了对模板有序性、孔径、膜厚度等的影响因素,总结出制备Al₂O₃有序膜的最佳工艺。     

高度有序氧化钨纳米棒的制备和表征

采用直流磁控溅射法结合阳极氧化法在铝基纳米点阵上制备氧化钨(WO3)纳米棒. 运用原子力学显微镜(AFM), 电子扫描显微镜(SEM), X射线衍射仪(XRD), 电化学工作站(EW)和紫外-可见分光光度计(UV)观察表征了WO3纳米棒的表面形貌、结构、光学性能和电致变色性能. 结果表明: 在溅射过程中, 溅射粒子优先沉积于铝基纳米点阵的凸点上, 然后成核并形成棒状; WO3纳米棒的直径约为200 nm, 与铝基纳米点阵的直径一致, 拥有一定的电致变色性能.     

取向碳纳米管/硅纳米线复合阵列的制备

在阳极氧化铝模板(AAO)的取向微孔内, 利用化学气相沉积(CVD) 技术首先制备了两端开口高度取向的碳纳米管阵列, 再在碳纳米管中间的孔洞内沉积硅纳米线, 成功制备了碳纳米管/硅纳米线(CNTs/SiNWs)核鞘复合阵列结构. 用SEM, TEM, XRD等仪器分析了CNTs/SiNWs核鞘复合阵列和沉积在碳纳米管孔洞内的硅纳米线的生长特性和晶体结构, 利用I-V关系和Fowler-Nordheim方程研究了其场发射(FE)特性, 用荧光光谱分析仪分析了复合阵列的荧光(PL)特性. 证明了模板法制备的CNTs/SiNWs核鞘复合阵列结构可用来制作具有金属/半导体(M/S)特性的纳米PN结, 该复合阵列结构也使SiNWs包覆在CNTs惰性鞘内, 可防止SiNWs在空气中的进一步氧化. 制备出的CNTs/SiNWs核鞘复合阵列结构生长方向高度有序, 直径和长度易于控制, 极少产生其他制备方法中出现的纳米结构弯曲和相互缠绕现象.     

铝阳极氧化膜阻挡层的去除方法

多孔型铝阳极氧化膜常被用作制备纳米阵列材料的模板,然而阻挡层的存在却在很多方面制约了其应用.为此,已经提出了各种不同的方法来去除阻挡层.本文将这些方法分为2类,即剥离氧化膜去阻挡层和不剥离氧化膜去阻挡层.前者包括化学腐蚀法、干蚀法、电解剥离法;后者包括阶梯降压法、高电流击穿法、电化学法和有多孔铝支撑的化学溶解法.其中,化学腐蚀法和干蚀法的工艺条件已相当成熟,得到了广泛应用,而其它几种方法还多处于实验室研究阶段.由于氧化膜脆性很大,因此,不剥离氧化膜原位去除阻挡层的方法具有更大的实用价值.     

b-轴取向MFI型分子筛膜制备工艺

6-轴取向MFI型分子筛膜是一种具有特殊纳米孔道结构的硅铝分子筛膜,在膜分离、膜反应器、化学传感器等领域有着广泛的应用前景,受到国内外学者的普遍关注.本文综述了b-轴取向MFI型分子筛膜制备工艺方面的研究进展,详细介绍了原位水热合成法和二次生长法制备工艺;重点总结和评价了近年来在载体表面修饰、b-轴取向分子筛晶种层制各...     

利用Fe3O4/DR膜作为催化剂前体在硅片上生长多壁碳纳米管

Fe3O4纳米粒子与正离子性的重氮树脂在硅基底的表面形成稳定自组装膜,还原后可通过化学气相沉积(CVD)法在硅基底的表面生长多壁碳纳米管.以聚丙烯酸包裹Fe3O4纳米颗粒能够有效地防止纳米粒子的团聚,并提高组装效率,得到均匀的纳米粒子自组装膜,从而获得在硅基底上均匀分布的多壁碳纳米管.     

L-胱氨酸在Pb/nanoTiO_2膜电极上的电催化还原

采用阳极氧化和恒电位沉积法制备Pb纳米粒子修饰的多孔Ti基TiO2(Pb/nanoTiO2)膜电极.通过对不同的电沉积电位和时间对比,找出了最佳电沉积条件.SEM分析显示该膜为均匀多孔结构,Pb纳米粒子均匀地分散在TiO2膜的表面.循环伏安和计时电流法研究了L-胱氨酸在Pb/nanoTiO2膜电极上的电催化还原活性,结果表明该电极对L-胱氨酸的还原具有高催化活性和稳定性.     

基于纳米CuZSM-5分子筛的传感器用于沙林检测的研究

将纳米ZSM-5或CuZSM-5分子筛作为敏感膜,结合石英晶体微天平(QCM)制备了对神经毒剂沙林(GB)敏感的传感器,研究了硅铝摩尔比和铜离子修饰对毒剂检测性能的影响.结果表明,硅铝摩尔比为25的纳米CuZSM-5分子筛对GB响应最好,并可对GB进行连续多次检测,其灵敏度为19.1 Hz/(mg·m-3),检出限达1.1 mg·m-3(S/N＝3);线性范围为1.5 ～20.0 mg·m-3,线性相关系数为0.995 8,在毒剂检测中具有较强的应用前景.     

Formation of gold-capped silicon nanocolumns on silicon substrate

Gold-capped silicon nanocolumns regularly distributed over silicon substrate were obtained. The columns length was roughly 100?nm; their deviation from perpendicular axis was less than 2°. The diameter of the columns was of the order of 10?nm or below of that. The proposed procedure of nanostructuring included the following main steps: deposition of aluminum thin layer (100?C500?nm) by magnetron sputtering on (100) oriented Si wafers; formation of porous self-ordered alumina structures by electrochemical anodizing of the Al film in oxalic acid; electroless inversion of Au in alumina pores; and reactive ion etching. The obtained Si?CAu structures are of importance as the platforms for biosensing applications, while the gold-free structures are of interest in photovoltaics.     

Formation of gold-capped silicon nanocolumns on silicon substrate

Gold-capped silicon nanocolumns regularly distributed over silicon substrate were obtained. The columns length was roughly 100 nm; their deviation from perpendicular axis was less than 2°. The diameter of the columns was of the order of 10 nm or below of that. The proposed procedure of nanostructuring included the following main steps: deposition of aluminum thin layer (100–500 nm) by magnetron sputtering on (100) oriented Si wafers; formation of porous self-ordered alumina structures by electrochemical anodizing of the Al film in oxalic acid; electroless inversion of Au in alumina pores; and reactive ion etching. The obtained Si–Au structures are of importance as the platforms for biosensing applications, while the gold-free structures are of interest in photovoltaics.

     

二次阳极氧化方法制备有序多孔氧化铝膜

通过二次阳极氧化方法制备多孔氧化铝膜与一次阳极氧化方法制备多孔氧化铝膜孔排布规律性的对比,结果发现,二次阳极氧化方法制取的多孔氧化铝膜孔排布规律性明显好于一次阳极氧化法制取的多孔膜.在几个微米范围内,孔呈理想的六角排布.去除一次阳极氧化膜后,二次阳极氧化得以在更良好的表面进行,制取的氧化铝膜孔规律性和有序度更高.有序区域的尺寸与晶粒内的亚晶大小有一定关系.     

Anodic alumina membranes with defined pore diameters and thicknesses obtained by adjusting the anodizing duration and pore opening/widening time

The through-hole porous anodic aluminum oxide (AAO) membranes were fabricated by a simple two-step anodization of aluminum in 0.3?M oxalic acid, 0.3?M sulfuric acid, and 2?wt.% phosphoric acid solutions under different operating conditions followed by the removal of the remaining Al substrate and the pore opening/widening process. The effect of duration of the second anodizing step on the thickness of the porous oxide layer and the influence of other anodizing conditions such as applied voltage, type of electrolyte, and purity of the substrate on the rate of porous oxide growth were discussed in detail. The pore opening procedure for all synthesized membranes was optimized, and the influence of the duration of chemical etching on structural features of AAO membranes, especially pore diameter, was studied. The rate of pore widening was established for AAO membranes formed in various anodizing electrolytes and for different temperatures of 5?wt.% H₃PO₄ used for alumina dissolution.     

Anodic alumina membranes with defined pore diameters and thicknesses obtained by adjusting the anodizing duration and pore opening/widening time

The through-hole porous anodic aluminum oxide (AAO) membranes were fabricated by a simple two-step anodization of aluminum in 0.3 M oxalic acid, 0.3 M sulfuric acid, and 2 wt.% phosphoric acid solutions under different operating conditions followed by the removal of the remaining Al substrate and the pore opening/widening process. The effect of duration of the second anodizing step on the thickness of the porous oxide layer and the influence of other anodizing conditions such as applied voltage, type of electrolyte, and purity of the substrate on the rate of porous oxide growth were discussed in detail. The pore opening procedure for all synthesized membranes was optimized, and the influence of the duration of chemical etching on structural features of AAO membranes, especially pore diameter, was studied. The rate of pore widening was established for AAO membranes formed in various anodizing electrolytes and for different temperatures of 5 wt.% H₃PO₄ used for alumina dissolution.

     

Synthesis and Characterization of Supported CuInSe2 Nanorod Arrays on Rigid Substrates

Copper indium diselenide nanorod arrays were electrodeposited on tungsten/silicon rigid substrates using porous anodic alumina as growth template. The porous anodic alumina templates were prepared by anodizing aluminum films which were sputtered onto the tung-sten/silicon substrates. A selective chemical etching was used to penetrate the barrier layer at the bottom of the alumina channels before electrodeposition, which enables direct elec-trical and chemical contact with the underside substrate electrode. The as-deposited sam-ples were annealed at 450 oC in vacuum. Scanning electron microscopy revealed that the nanorods were dense and compact with diameter of about 100 nm, length of approximate 1 μm, and the aspect ratio of 10. X-ray diffraction, micro-Raman spectroscopy, and highresolution transmission electron microscopy showed that chalcopyrite polycrystalline struc-ture and high purity CuInSe₂ nanorods were obtained. The grain size was large in the rod axial direction. Energy-dispersive X-ray spectroscopy showed the composition was nearly stoichiometric. The energy band gap of this nanorod arrays was analyzed by fundamental absorption spectrum and was evaluated to be 0.96 eV.     

铝的多孔阳极氧化自组织过程结晶度依赖特性

电子束蒸发在硅衬底上的多晶铝膜多孔型阳极氧化得到的多孔列阵排布与体材料单晶铝氧化结果比较,有序度存在很大差异,导致这种差异的原因,除了氧化时间、应用电压、电解液等电化学参数外,新引入的结晶度将作为一重要因数影响自组织过程.结晶度的影响主要反映在晶粒间界区域相比于晶粒内部存在的铝原子浓度和阳极氧化反应速度涨落,这种涨落将通过干扰孔底电场的分布,对自组织过程产生微扰,由于微扰具有实时和随机性质,将使铝膜阳极氧化不再象体材铝那样,可以通过单一延长时间来最终改善孔排布的有序度.     

多孔阳极氧化铝膜的制备研究

在直流恒压下,在不同的酸性溶液中对铝片实施两步阳极氧化制备多孔氧化铝膜,在磷酸溶液中制得的模板孔径大,并且电解时间缩短,加快了制备模板的过程。同时利用阳极氧化初期电流密度的变化,分析了多孔氧化铝膜的形成机理。     

纳米孔阵列阳极氧化铝膜的制备和表征

本文通过在0℃、0.5mol·L^-1的草酸溶液中阳极氧化高纯铝片的方法制得了阳极氧化铝(AAO)膜，并用扫描电子显微镜(SEM)和原子力显微镜(AFM)对AAO膜的形貌和结构进行了表征。结果表明，阻挡层AAO膜中大小一致的膜胞在铝/氧化铝界面上排成六方形阵列;有孔层AAO膜中含有高度有序的纳米孔阵列和膜胞阵列，并且孔的直径和膜胞的尺寸都具有较窄的分布。另外，考察了阳极氧化电压对膜胞尺寸、孔径大小、孔密度和膜胞密度的影响，表明在一定的电压范围内，膜胞和孔径都随电压的升高而增大，而孔密度和膜胞密度却随电压的升高而减小。     

Highly increased breakdown potential of anodic films on aluminum using a sealed porous layer

The growth of a uniform barrier-type anodic film on aluminum is usually terminated by electric breakdown, which is controlled by the resistance of electrolyte or anion concentration. In this study, highly resistive porous layers have been introduced by anodizing aluminum in sulfuric acid electrolyte followed by boiling water treatment to examine their influence on the electric breakdown potential. The pores of the porous alumina film are sealed by forming hydrated alumina (pseudo-boehmite) after the boiling water treatment. The breakdown potential increases to over 1500 V for the pore-sealed aluminum specimens on anodizing in sodium tungstate electrolyte. The electrochemical impedance spectroscopy measurements revealed an increased resistance of the porous layer after the pore-sealing treatment. GDOES depth profile analysis disclosed that the sealed porous layer impedes the incorporation of tungsten species into the barrier layer. The introduction of a highly resistive layer that also suppresses the anion incorporation on aluminum is effective in increasing the breakdown potential of anodic films.