电化学沉积金纳米线结构及其电学特性

用电化学沉积方法，在有机介孔模板上制备出直径为90 nm的金纳米线.透射电子显微镜（TEM）分析结果表明，纳米线表面光滑并呈单晶结构.去除有机模板的金纳米线阵列用扫描电子显微镜（SEM）测试，纳米线顶端呈平台状，直径分布均一.我们利用原子力显微镜（AFM）测量了金纳米线阵列的微观结构，得到与SEM相一致的结果.在大气和室温条件下，用导电AFM针尖在接触模式下测量了单根纳米线的轴向I－V特性曲线，其结果为金属性.     

金纳米线阵列制备及其光谱特性

利用电化学沉积方法在重离子径迹模板中制备出直径从45 nm到200 nm, 长径比达700的金纳米线阵列, 利用扫描电子显微镜(SEM)和X射线衍射(XRD)对所制备金纳米线的形貌及晶体结构进行分析, 结果表明, 在1.5 V(无参比电极)沉积电压下所制备出的直径为200 nm金纳米线沿[100]晶向具有较好择优取向. 利用紫外-可见光谱(UV-Vis)对镶嵌在透明模板中平行排列的金纳米线阵列光学特性进行研究, 发现金纳米线直径为45 nm时, 其紫外可见光谱在539 nm处有强烈吸收峰, 随着金纳米线直径增加, 吸收峰红移, 当金纳米线直径达到200 nm时, 其吸收峰峰位移至700 nm. 结合金纳米颗粒相关表面等离子体共振吸收效应对实验结果进行了讨论.     

纳米金、碳纳米管和纳米线及其在电化学生物传感器研究中的应用

综述了1995～2007年间,纳米金、碳纳米管和纳米线材料及其在电化学生物传感器研究中的新进展,引用文献60篇.     

单根TiO2纳米线一维电子输运性能

采用电化学诱导溶胶-凝胶法, 在多孔氧化铝模板(AAO)的纳米孔道内制备了直径分别为60 和20 nm的锐钛矿型TiO₂纳米线阵列. 利用原子力显微镜(AFM)技术, 在半接触模式下得到了TiO₂纳米线的形貌像, 在接触模式下测量了单根TiO₂纳米线的I-V曲线. TiO₂纳米线的电子输运性能表现为半导体的性质. TiO₂纳米线的导通电压值明显小于TiO₂块体,并且随着TiO₂纳米线直径的减小, 导通电压值增大.     

Mg掺杂GaN纳米线的结构及其特性

利用类似Delta掺杂技术在硅衬底上沉积Mg:Ga2O3薄膜, 然后在850 ℃下对薄膜进行氨化, 反应后制备出大量Mg掺杂GaN纳米线. 采用扫描电子显微镜(SEM)、X射线衍射(XRD)、傅里叶变换红外(FTIR)光谱和高分辨透射电子显微镜(HRTEM)对样品进行分析.结果表明, Mg掺杂GaN纳米线具有六方纤锌矿单晶结构, 纳米线的直径在30-50 nm范围内, 长度为几十微米.     

以金纳米颗粒-二氧化钛纳米线阵列为支架的电化学免疫传感的构建及其应用

首先以掺杂氟的二氧化锡导电玻璃为基片,采用水热法制备出二氧化钛纳米线阵列,然后使用电化学沉积法将金纳米颗粒修饰于二氧化钛纳米线阵列表面以增强其导电性和生物相容性.将纳米金-二氧化钛纳米线阵列用作电化学免疫传感器支架,利用纳米金与癌胚抗原抗体之间的静电吸附作用,将包被抗体负载于电极表面制得检测癌胚抗原的电流型免疫传感器.同样,水热法还被用于制备圆柱形二氧化钛纳米棒,以辛二酸双(3-磺基-N-羟基琥珀酰亚胺酯)钠盐为双氨基交联剂,将辣根过氧化物酶和信号抗体一起固定于二氧化钛纳米棒表面作为示踪标记物.扫描电子显微镜、透射电子显微镜和X射线衍射分析仪均被用于分析上述材料的结构、形貌和组成.通过夹心型免疫反应,示踪标记物上信号抗体被定量负载于免疫传感器表面.通过一个以过氧化氢为媒介体的辣根过氧化物酶催化反应,差示脉冲伏安法被用于癌胚抗原的定量测定.结果表明,该癌胚抗原免疫传感器线性范围为0.01~120μg/L,检测限为6 ng/L.     

低频交流电沉积金纳米线阵列的AFM研究

迄今,人们已采用许多方法制备纳米材料,如刻蚀技术、化学法和模板法等［1]．其中,引起科学界广泛兴趣的模板法,在合成有序纳米材料上占有极其重要的地位．常用的模板有两种,一种是有序孔洞阳极氧化铝（Anodic Aluminum Oxide,AAO）模板[2],另一种是含有孔洞无序分布的高分子模板．AAO模板具有耐高温,绝缘性好,孔洞分布均匀有序,而且大小可控等特点［3]．可以利用 AAO模板来制备各种纳米纤维和纳米管,如导电聚合物［4]、金属［5]、半导体［6]、碳［7]和其它一些材料．由于纳米材料的应用具有广阔的前景,如光催化、电化学、酶固定等方面,因而不同材料纳米线的制备备受关     

电化学法制备硅纳米线

Silicon nanowires were synthesized from nanometer silicon dioxide powder under potentiostatic electrolysis at -1.20 V (vs Pt reference) for 4 h in molten CaCl₂ at 900 ℃. The morphology, structure and chemical composition of the samples prepared by electroreduction method were characterized by field-emission scanning electron microscopy(FE-SEM), High-resolution transmission electron microscopy(HRTEM) coupled with electron energy dispersive spectroscopy(EDS), laser Raman and X-ray diffraction(XRD). The results revealed that silicon nanowires were crystalline with a diamond cubic structure, the diameter was distributed from 50 nm to 80 nm and the length was generally several micrometers. The formed nanowires basically consisted of silicon monocrystalline and amorphous oxide sheath.     

一步湿化学法合成超细金纳米线

以氯金酸(HAuCl₄)为前驱物, 油胺同时作为溶剂、表面稳定剂和还原剂, 通过简单的一步湿化学法合成超细金纳米线. 制备出的超细金纳米线不仅产量高、纯度高, 而且纵横比大, 纳米线平均直径~2 nm, 长度可达数十微米. 如果添加另一种还原剂油酸并调节油胺和油酸的体积比为1:1, 将生成直径为~9 nm的金纳米线. 通过改变反应温度和还原剂用量, 对该种超细金纳米结构的生长机制进行阐述说明: 以油胺为模板, 在油胺和一价金卤化物(AuCl)亲金键合形成的一维聚合链作用下, 被还原的金原子附着在已成核颗粒表面, 一维地生长成超细金纳米线.     

用金纳米粒子修饰硅纳米线及复合结构的光谱性质研究

在溶液中以正己硫醇作稳定剂, 利用HAuCl4与HF处理后的硅纳米线(SiNWs)的氧化还原反应, 在SiNWs表面负载金纳米粒子(AuNPs). 通过调整HAuCl4的浓度, 得到了AuNPs粒径从3.2到7.0 nm的AuNPs/SiNWs复合结构, 并对这种复合结构进行了紫外-可见吸收光谱和荧光光谱研究. 紫外-可见吸收光谱研究表明, 负载不同粒径的AuNPs的SiNWs在530～580 nm间有明显的由AuNPs表面等离子体共振引起的吸收, 且随着AuNPs粒径的增加, 该吸收峰发生红移. 负载前后的荧光光谱表明, 在红光和绿光区负载AuNPs的SiNWs的荧光峰与HF处理后SiNWs的荧光峰峰形相当, 峰位变化不大; 但在蓝光区, 不同于HF处理前后SiNWs的发射峰(464 nm左右), 负载了AuNPs的SiNWs在423 nm的位置处出现了强荧光峰, 这个峰是AuNPs费米能级的电子与sp或d带的空穴辐射复合产生的.     

电化学沉积金锡合金及其性能研究

以柠檬酸金钾和氯化亚锡为主要原材料,配制Au~+及Sn~(2+)浓度分别为8 g/L和10 g/L的溶液,在不同电流密度下通过电化学沉积获得金锡合金镀层。通过X-射线衍射(XRD)、扫描电子显微镜(SEM)、微区元素成分分析(EDS)及差示扫描量热分析(DSC)等手段对镀层的物相、微观形貌、金含量及熔融性能进行了系统研究。结果表明,电流密度0.030～0.045 mA/mm~2为最佳电流密度范围,可获得熔融温度约280℃、焊接性能良好的金锡合金镀层。     

Formation and Characterization of Europium Bisphthalocyanine Organic Nanowires by Electrochemical Deposition

Europium bisphthalocyanine (EuPc2) nanowires were prepared by electrochemicaldeposition method. Scanning electron microscopy (SEM) images show the evolution of themorphologies of nanowires obtained under different deposition time (Td). The optical properties ofeuropium bisphthalocyanine films were studied by UV-Vis absorption spectra. The morphology of EuPc2 nanowires could be controlled by changing deposition conditions, which provides a usefulmethod to make organic nanowires.     

Luminescence Property and Synthesis of Sulfur-doped ZnO Nanowires by Electrochemical Deposition

"Sulfur-doped zinc oxide (ZnO) nanowires were successfully synthesized by an electric field-assisted electrochemical deposition in porous anodized aluminum oxide template at room temperature. The structure, morphology, chemical composition and photoluminescence properties of the as-synthesized ZnO:S nanostructures were investigated. X-ray diffraction and the selected area electron diffraction results reveal that the as-ynthesized products are single phase with hexagonal wurtzite structure with a highly preferential orientation in the (101) direction. Transmission electron microscopy observations indicate that the nanowires are niform with an average diameter of 70 nm and length up to several tens of micrometers. X-ray photoelectron pectroscopy further reveals the presence of S in the ZnO nanowires. Room-temperature photoluminescences observed in the sulfur-doped ZnO nanowires which exhibits strong near-band-edge ultraviolet peaks at 378 and 392 nm and weak green emissions at 533 and 507 nm. A blue emission at 456 nm and violet emissions at around 406, 420, and 434 nm were also observed in the PL spectrum for the as-synthesized ZnO:S nanowires. The PL spectrum shows that S-doping had an obvious effect on the luminescence property of typical ZnO nanowires."     

以DNA为模板构造苯胺-DNA复合物纳米线和聚苯胺纳米导线

在溶液中, 以DNA为模板构造出了线性的苯胺-DNA复合物纳米线. 用压缩气流将得到的复合物纳米线拉直并固定到云母基底上. 用原子力显微镜(AFM)可观察到形貌规整的苯胺-DNA复合物纳米线. 苯胺单体在溶液中能从各个方向上组装到DNA分子上, 从而使DNA模板分子的表面包裹了一层苯胺. 以苯胺-DNA复合物纳米线为前驱体通过进一步化学氧化聚合得到了以DNA为模板的聚苯胺纳米导线.     

Electrochemical Deposition and Spectroelectrochemical Response of Bromophenol Blue Films on Gold

Bromophenol blue (BPB) was electropolymerized onto a Au substrate. The effects of voltammetric cycle number, BPB concentration, and pH on film thickness, density, optical absorption, and electrochemical susceptibility were evaluated, and favorable deposition conditions were identified. Quantitative measurement of the film mass via quartz crystal microbalance enabled determination of the molar volume and revealed a strong dependence of film density with deposition pH. Finally, electrochemical control of the optical properties of BPB films was demonstrated via in situ spectroelectrochemistry. We believe this is the first demonstration of electropolymerization of pure BPB on Au, and thus the first demonstration of poly(BPB) as an electrochemically switchable optical coating.     

自组装金电极的电化学测试及其FTIR和AFM分析

利用交流阻抗谱测试了自组装免疫电极的抗原响应特性，对生物电极解离过程的机理进行了研究，用傅里叶变换红外反射光谱（FTIR）和原子力显微镜（AFM）对电化学实验过程进行了直观观测和定量分析。     

Field Emission and Superhydrophobic Properties of Electrochemically Grown Gold Nanourchins

We demonstrate a convenient fabrication of Au nanourchins (NUs) on Si substrates via a surfactant‐assisted galvanic reduction process. This synthetic method not only grows Au NUs on Si in a one‐step process but also effectively controls the lengths of the branches on the NUs. The widths are about 100‐120 nm and the lengths can be extended from 200 nm to 5 μm by lengthening the growth time. With the advantage of a hierarchical surface structure, Au NUs exhibited excellent electron field emission (FE) performance (turn‐on voltage, 6.3 V/μm; β, 1150). In addition, the wetting behavior examination shows that the water contact angle can be as high as 158° on Au NUs after the material is treated by 1‐hexadecanethiol.     

Highly Selective Nanostructured Electrochemical Sensor Utilizing Densely Packed Ultrathin Gold Nanowires Film

The number of studies conducted about nonenzymatic electrochemical sensors has increased in recent years due to the development of more stable and robust electrodes using noble metals. One of the key aspects for achieving high sensing performance including detection limit and sensitivity is the design of electrode architecture. Herein, we report a new electrochemical sensing platform featuring ultrathin standing gold nanowires (AuNWs) for nonenzymatic detection of hydrogen peroxide (H₂O₂). The use of AuNWs resulted in an increased electron transfer efficiency due to the higher active surface area compared to traditional gold film electrodes. This sensor demonstrates good selectivity, reproducibility, a linear range up to 49.5 mM of H₂O₂ with a sensitivity of 0.185±0.003 mAmM^?1cm^?2 and a limit of detection of 111 μM. The biological relevance of this sensor was tested in cell culture media to illustrate the performance of the proposed sensing electrode in complex biological media.     

云母晶面上准外延生长的胶原蛋白纳米线阵列的性质研究

胶原蛋白纤维与同样具有周期性结构表面的羟磷灰石等矿物质晶体能够通过多种作用在介观尺度上相互识别,从而有效地进行规范骨骼、牙齿等器官生长的生物矿化.在本研究中,反相利用生物矿化原理,开发出一种与热壁外延生长(Hot wall epitaxy)技术效果相似的生物大分子纳米线阵列的简单制备技术,成功地将5～10 μg/mL的天然I型鼠尾胶原蛋白单体溶液在云母晶体的(001)晶面上培育成取向单一且长程有序的胶原蛋白纳米线阵列.原子力显微镜实验结果表明,纳米线阵列随胶原蛋白单体浓度增大而变得致密,但是单条纳米线的宽度与高度较为稳定,分别约为60.0和1.5 nm.有纳米线覆盖的云母晶面亲水性好,晶面接触角由25.8°降为9.5°.基于电子背面散射衍射和透射电子显微镜的分析表征结果,纳米线的取向应沿云母[110]方向, 更详实地验证了胶原蛋白纳米线的准外延生长机理.