恒电流密度法制备大孔径高度有序阳极氧化铝模板

采用恒电流密度法,分别在草酸和磷酸的电解液中制备了阳极氧化铝模板(AAO),借助扫描电镜(SEM)观察了膜的微观形貌,结合恒电压法制备的AAO模板,研究了电解液、电流、电压等对膜的影响,并且探讨了恒电压和恒电流密度法的形成机理.结果表明:利用恒电流密度法制得的模板孔径大约在80～200nm,厚度在30～100μm,并且孔径均匀,有序性好.     

纳米氧化铝有序多孔膜制备工艺研究

为了获得大面积有序孔排列以及不同孔径的氧化铝膜,采用二次阳极氧化法可制备大面积有序铝阳极氧化多孔(AAO)膜,着重研究氧化电压、氧化时间、电解液浓度以及扩孔时间对AAO膜孔径大小、膜层厚度和形貌结构的影响,用X射线粉末衍射(XRD)仪进行物相分析,利用扫描电子显微镜(SEM)表征多孔膜的形貌.结果表明,在700 ℃以下条件下AAO膜以无定形态存在,经800 ℃退火后无定形氧化铝转化为γ-Al2O3,多孔膜随电压和电解液浓度增加而增大,经H3PO4溶液扩孔后可获得较大孔径模板,扩孔时间与孔径变化呈近似线性关系.为满足应用需求的AAO膜的制备提供了依据.     

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。     

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.     

大内径碳纳米管的制备研究

采用化学气相沉积法（chemical vapor deposition）制备碳纳米管．在高温裂解甲烷制备碳纳米管的反应体系中，比较研究了碳酸钠、碳酸钾、碳酸钙和碳酸钡等碳酸盐作为毒物对镍基催化剂和碳纳米管的影响；另外，还考察了裂解温度对碳纳米管的产率和管型的影响。实验中采用气相色谱（gas chromatography）在线检测甲烷的转化率，从而比较镍基催化荆的催化活性；采用透射电子显微镜（transmission electron microscopy）对合成的碳纳米管的外部形貌进行观察。结果发现，无论是从碳纳米管的产率还是形貌，碳酸钠均优于其它几种碳酸盐，内管径可达到70-80nm，另外还发现，750℃为此法制备碳纳米管的最佳裂解温度。     

草酸/磷酸混合介质制备高质量阳极氧化铝模板

以草酸为主导酸、磷酸为辅助酸的混合介质作为电解液,采用不对称二次氧化法制备阳极氧化铝模板(AAO模板),通过调节电压、介质配比和酸的浓度等方式研究其生长机制及优化条件.利用扫描电子显微镜(SEM)和电流监测装置对得到的AAO模板进行表征,结果表明在低压(40 V)、较低浓度草酸条件下,适量掺杂磷酸可以提升模板阵列有序性、孔洞规则性及孔径;在高压(80 V)下制备出表面具有V字型结构孔洞的模板,当混合介质中主导酸和辅助酸各自适配电压与施加电压差值比为其混合体积比倒数时所制备的模板质量最优,且随电压增大V字型结构的孔径增大,但辅助酸掺杂量不宜过高.本研究可为采用多元介质制备大孔径优质AAO模板提供参考.     

ZrO2纳米管的溶胶-凝胶模板法制备与结构表征

用溶胶-凝胶法在多孔阳极氧化铝模板中制备了ZrO2纳米管.通过SEM和TEM表征了ZrO2纳米管的形貌,用选区电子衍射和XRD研究了ZrO2纳米管的晶体结构,FT-IR分析了zrO2纳米管的键合结构.结果表明,所制备的纳米管阵列高度有序,管径和长度分别与AAO模板的孔径和厚度相当;纳米管管壁的厚度随浸泡时间增加而增厚,可通过控制浸泡时间等因素来制备不同孔径的纳米管或线.ZrO2纳米管为单斜晶和立方晶形的多晶结构;纳米管的形成机理是溶胶粒子在AAO模板孔壁酸位上的吸附.     

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。     

两次氧化条件对阳极氧化铝孔洞的影响

采用两次阳极氧化法在草酸溶液中制备多孔氧化铝(AAO),分别研究了电压、氧化时间及草酸溶液浓度对AAO孔洞特征的影响。结果表明,在第一次氧化过程中孔间距随氧化电压的提高而增大,氧化时间和草酸溶液浓度几乎没有影响;在第二次氧化过程中时间、电压及草酸溶液浓度对孔间距基本无影响,但是随着氧化电压的增大AAO孔径明显增大,孔洞呈六方阵列排布。此外,第二次氧化电压增大时孔洞形状由圆形到长条形、再到六边形变化;第二次氧化草酸溶液浓度增大至0.4 mol/L时所制备的AAO的相邻孔洞沿特定取向发生贯穿现象,甚至溶解,而孔洞整体分布有序性几乎不受影响。     

结合溶胶-凝胶和微波法制备二氧化钛纳米管

以溶胶-凝胶法制备得到的TiO_2纳米粉体为原料,采用微波法制备TiO_2纳米管,用透射电子显微镜和扫描电子显微镜对纳米管和纳米粉体进行表征,结果表明,制得的TiO_2纳米管形貌比较完整,其外径为8-15nm、内径为5-10nm、长50-100nm,同时发现,未经HCl酸洗的TiO_2纳米管在电镜下非常完整,而经过HCl酸洗的TiO_2纳米管则局部遭到破坏。     

Effects of sodium content of titanate nanotubes on lithium battery performance

Titanate nanotubes were prepared by hydrothermal process of powder for the application to the anode of lithium batteries. After the synthesis of titanate nanotubes by the chemical treatment with 10 M NaOH solution, the quantity of sodium remnant was controlled by the HCl washing solutions of different pH of 1, 4, 7, 10 and 13. The prepared titanate nanotubes had outer and inner diameter of 9 nm and 6 nm, and the interlayer spacing of about 1 nm. The amount of sodium remnant was investigated using Inductively Coupled Plasma (ICP) Atomic Emission Spectrometer, and the variation of structure and morphology with the contents of the sodium was studied by X-ray diffraction (XRD), Thermogravimetric Analysis (TGA), Field Emission Scanning Electron Microscopy (FE-SEM) and High Resolution Transmission Electron Microscopy (HR-TEM). Coin cells composed of (Titanate nanotubes//1 M LiPF6-EC/DEC//Li metal) were prepared for studying the basic charging-discharging behavior and electrochemical properties of the prepared titanate nanotubes with controlled sodium contents. The effects of the remnant sodium content on the microstructures, morphology and electrochemical properties of titanate nanotubes will be discussed.     

高长径比TiO_2纳米管的制备及表征

用钛粉为原料,在强碱性条件下,用简单的水热方法制备出了大量高长径比的TiO2纳米管。讨论了对前驱物钛粉进行热处理对TiO2纳米管结构的影响。在热处理温度为800℃的条件下制备出了外径约为10nm,内径约为5nm,平均长度为3μm的TiO2纳米管。用扫描电子显微镜、X-射线衍射,透射电镜分别表征了TiO2纳米管的微观形貌,成分与结构。     

微纳分级结构碳酸钙中空微球的可控制备

以CaCl₂和Na₂CO₃为反应原料, 以聚乙烯吡咯烷酮(PVP)和十二烷基磺酸钠(SDSN)为模板剂, 在50℃采用化学沉淀反应, 干燥、煅烧后成功制备了具有微纳分级结构的CaCO₃中空微球。采用扫描电子显微镜、透射电子显微镜和X射线衍射等检测手段对所制备的样品形貌、结构进行了表征, 结果显示：所制备的微纳分级结构CaCO₃中空微球直径为4~6 μm, 壳壁由直径约60 nm的CaCO₃颗粒组成, 壳层厚度约为200 nm, CaCO₃中空微球晶相组成为方解石和球霰石的共混体。同时, 在反应温度为50℃、PVP添加量为0.4 g, SDSN浓度为0.1 mol/L的条件下, 所制备的微纳分级结构CaCO₃中空微球分散性好, 且形貌比较完整。     

Fabrication, structural characterization and formation mechanism of multiferroic BiFeO3 nanotubes

Multiferroic BiFeO3 (BFO) nanotubes have been successfully fabricated by the modified sol-gel method within the nanochannels of porous anodic aluminum oxide (AAO) templates. The morphology, structure and composition of the nanotubes were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), selected-area electron diffraction (SAED), high resolution TEM, (HRTEM) and energy-dispersive X-ray spectroscopy (EDX). Postannealed (650 degrees C for 1 h), BFO nanotubes were polycrystalline and X-ray diffraction study revealed that they are of the rhomohedrally distorted perovskite crystal structure. The results of SEM and TEM revealed that BFO nanotubes possessed a uniform length (up to 60 microm) and diameter (about 200 nm), which were controlled by the thickness and the pore diameter of the applied AAO template, respectively and the thickness of the wall of the BFO nanotube was about 15 nm. Y-junctions in the BFO nanotubes were observed. EDX analysis demonstrated that stoichiometric BiFeO3 was formed. HRTEM analysis confirmed that the obtained BFO nanotubes made up of nanoparticles (3-6 nm). The possible formation mechanism of BFO nanotubes was discussed.     

微波水热法合成钛酸钠盐纳米管

采用微波水热法合成了钛酸钠盐纳米管,考察了原料、反应时间、NaOH浓度等主要影响因素.在微波功率195W、NaOH浓度8—12mol/L、反应时间>70min条件下,得到了形貌均一的钛酸钠盐纳米管,并用TEM、XRD、BET、EDAX和N₂吸附/脱附等对产物进行了表征.研究表明,微波法制得的纳米管合成时间短、热稳定性高,其管壁塌陷温度高于500℃,比普通水热法合成的高100℃左右;所得样品在300℃以上煅烧,可转化为单晶钛酸纳盐纳米管.     

Facile fabrication of nickel phosphate nanotubes via a urea-assisted hydrothermal route

Nickel phosphate nanotubes (NiPO-NTs) were obtained via a simple urea-assisted hydrothermal route in the absence of organic surfactant as the structure-directing agent. The material possessed an urchin-shaped structure, and the one dimensional nanotubes were directed outward around the spheres. SEM and TEM observations indicated that the NiPO-NTs had an outer diameter of about 7.0 nm, inner diameter of 4.0 nm, and length of around 0.75 μm. It is found that the formation of NiPO-NTs was determined by the pH value and its changing rate, which were controlled by urea hydrolysis. Accordingly, a possible mechanism of nanotube formation was proposed. The synthesized NiPO-NTs showed high catalytic performance in the epoxidation of cyclohexene.     

氰化滚镀铜工艺实践与探讨

氰化滚镀铜溶液中碳酸钠含量和主盐浓度不当,都会影响产品的质量.影响碳酸钠含量的因素较多,如溶液的pH值及NaOH浓度,槽电压等.对其具体影响进行了研究,提出措施:NaOH浓度在5.0～7.5 g/L可以将碳酸钠浓度控制在工艺范围内;降低镀槽电压和增加阳极面积有利于降低碳酸钠的浓度;较高的主盐浓度可以提高镀液的电流效率和均镀能力,有利于降低电镀成本.     

Fabrication of polystyrene/gold nanotubes and nanostructure-controlled growth of aluminate

Direct adsorption of gold nanoparticles in the inner of alumina template and following immersion of polystyrene (PS) dichloromethane solution in the template resulted in the fabrication of composite nanotubes of PS and gold nanoparticles. Several methods have been used to characterize the tubular structure. Nanostructured sodium aluminates were formed when the anodic alumina oxide membrane was dissolved by the sodium hydroxide. A "flower" shape was found after etching the template while the synthesis process was recorded as function of a time. The results demonstrate that the shape and size of the aluminates nanostructure can be controlled by etching time and the pore diameter of the alumina membrane.