多孔硅上银纳米粒薄膜的制备及其表面增强红外光谱

通过简便的化学沉积法在多孔硅上制备银纳米粒薄膜用于表面增强红外光谱检测。通过Ag⁺与多孔硅表面的SiHx发生氧化还原反应将银纳米粒子沉积在多孔硅表面。红外探针分子溶解于无水乙醇中进而被均匀分散在多孔硅表面,实验结果显示：对氨基苯硫酚、对氨基苯甲酸和对氟苯硫酚3个探针分子的红外峰分别最大增强了10、85和21倍。银纳米粒的大小和形状等物理特性、探针分子是否有与银表面进行强结合的基团和芳烃结构、以及表面选律等因素影响表面增强红外的吸收效应。     

微结构化弹性体介电层的制备方法与应用

微结构化弹性体薄膜是指在表面或内部具有多孔或者特殊造型阵列的微纳米尺寸结构的弹性体薄膜,这类薄膜作为功能化介电层在柔性电子器件的制备领域获得了广泛的应用。本文从微结构弹性体介电层的制备和应用两个方面来介绍微结构弹性体介电层的研究进展,首先介绍了可用以制备介电层的弹性体的种类,然后综述了多孔和非多孔阵列两大类微结构弹性体介电层的制备方法(氯化钠模板法、糖模板法、碳酸氢盐类模板法、微球模板法和硅模板法等);并介绍了微结构弹性体介电层在应力应变传感器和纳米发电机上的应用。     

电沉积法制备固态染料敏化太阳能电池

本文采用一步电化学沉积的方法在导电玻璃上先后沉积了ZnO/染料复合薄膜以及CuSCN薄层,实现仅以电沉积法制备结构为ZnO/染料/CuSCN的固态染料敏化太阳能电池,电池的光电转换效率达到0.1%.在电沉积CuSCN前,脱附电沉积制备的ZnO/染料复合薄膜中的染料以形成多孔ZnO薄膜,然后通过染料再吸附得到染料敏化ZnO纳晶多孔薄膜.在电沉积过程中,ZnO和CuSCN的晶体尺寸、晶体取向和膜层形貌都可以进行比较精准的控制.探讨了影响沉积薄膜形貌和光电转换效率的因素,如旋转圆盘电极的旋转速度、电沉积温度以及染料敏化剂的选择.本文报道的低温电沉积制备全固态太阳能电池的方法为制备柔性染料敏化太阳能电池提供了一种新的思路.     

氢气泡模板法电沉积制备三维多孔铜薄膜

应用阴极析氢气泡模板法电沉积制备三维多孔铜薄膜,基础电解液组成为0.2 mol.dm-3CuSO4和1.5 mol.dm-3H2SO4.研究了电流密度(0.5~8.0 A.cm-2)、温度(20~70℃)、支持电解质(Na2SO4)以及添加剂HC l和聚乙二醇(PEG)等对薄膜的孔径大小和孔壁结构的影响.扫描电子显微镜(SEM)分析表明,降低镀液温度和添加Na2SO4、PEG都可降低孔径的大小,但对孔壁结构无影响.加入微量的氯离子可显著改变薄膜的孔壁结构,得到孔壁结构较为致密的三维多孔铜电极.循环伏安(CV)测试结果显示三维多孔铜薄膜电极在碱性条件下电氧化甲醇的电流密度比光滑铜电极提高了近20倍.     

铂和钌纳米薄膜电极的全湿法制备及表面增强红外效应

金属纳米薄膜的合理制备是衰减全反射表面增强红外光谱法(ATR-SEIRAS)成功应用的关键. 通过简便可控的全湿法镀膜, 即先在红外窗口硅面上化学镀金膜, 而后再电沉积铂或钌, 制得具有极强表面增强红外效应、吸收峰向正常且几乎“无针孔”的铂或钌纳米薄膜电极, 从而可使ATR-SEIRAS技术广泛应用于研究铂、钌电极表面的吸附与反应.     

氧化钒/多孔硅/硅结构的微观形貌、纳米力学及温敏特性

采用电化学腐蚀法在硅基片表面形成多孔硅, 利用直流对靶反应磁控溅射方法在不同电流密度条件下制备的多孔硅样品表面上溅射沉积了VOx薄膜, 获得了氧化钒/多孔硅/硅(VOx/PS/Si)结构. 采用场发射扫描电镜(FESEM)观测多孔硅及VOx/PS/Si结构的微观形貌, 采用纳米压痕仪器测量VOx/PS/Si结构的纳米力学特性, 通过电阻-功率曲线分析研究其温度敏感特性. 实验结果表明, 在40和80 mA·cm-2电流密度下制备多孔硅的平均孔径分别为18和24 nm, 用显微拉曼光谱法(MRS)测量其热导率分别为3.282和1.278 kW·K-1; VOx/PS/Si结构的电阻随功率变化的平均速率分别为60×10⁹和100×10⁹ Ω·W-1, VOx/PS/Si结构的显微硬度分别为1.917和0.928 GPa. 实验结果表明, 多孔硅的微观形貌对VOx/PS/Si结构的纳米力学及温敏特性有很大的影响, 大孔隙率多孔硅基底上制备的VOx/PS/Si 结构比小孔隙率多孔硅基底上制备的具有更高的温度灵敏度, 但其机械稳定性也随之下降.     

硅片表面多金属污染的交流阻抗表征

在接近氢氟酸实际应用浓度条件下, 利用交流阻抗技术研究了硅片表面金属微观污染行为, 在氢氟酸溶液中分别加入0.5和1 mg/g的铜、铁、镍、钙四种金属离子, 获得了硅片在单金属溶液中的特征交流阻抗谱, 并在此基础上研究了三种金属及四种金属共存时的特征交流阻抗谱, 通过等效电路的拟合估算了硅/氢氟酸界面电化学反应的动力学参数, 并结合扫描电镜形貌图探讨了不同类型的单金属和多金属对硅电化学行为的影响. 结果表明, 多金属微观污染是各种单金属协同作用的结果, 铜在硅片上发生电化学沉积, 直接导致硅片表面粗糙化. 铁对硅片表面的破坏严重, 同时影响铜的沉积. 镍的存在使硅片表面更容易氧化. 而钙通过在硅片表面形成氟化钙沉淀物可以钝化表面, 减缓铜在硅片表面的沉积.     

激光刻蚀模板中电沉积特殊结构CIGS薄膜

本文利用激光刻蚀模板,在水溶液中电沉积制备金属铜薄膜,讨论了温度、电流、硫酸铜浓度对薄膜形貌的影响. 采用SEM对制备的铜薄膜进行表征,结果表明在沉积温度为30 ℃,沉积电流为4 A·dm^-2(表观工作电流密度),硫酸铜浓度在20 ~ 50 g·L^-1的水溶液中电沉积可以得到中空馒头状和开口碗状结构的铜薄膜. 利用激光刻蚀模板,在离子液体1-丁基-3-甲基咪唑三氟甲磺酸盐([BMI][TfO]) - 30 Vol%丙醇混合电解质中电沉积CIGS薄膜,研究了沉积电势、沉积时间对薄膜形貌的影响. SEM观察发现,在沉积电势为-1.8 V,沉积时间为1.5 h条件下电沉积可以得到近似柱状的簇状花束样的CIGS薄膜, 电沉积铜后再进一步电沉积CIGS,得到了均匀有序的鼓包柱状结构的Cu/CIGS复合薄膜. 用恒电势方波法对制备的薄膜真实表面积进行测试,计算结果表明,与无模板电沉积制备的CIGS薄膜相比,激光刻蚀模板法制备的Cu/CIGS复合薄膜的表面积提高了约8倍.     

电化学阻抗谱法研究温度对三维多孔Cu6Sn5合金电极嵌锂过程的影响

采用氢气泡为动力学模板电沉积获得多孔铜,通过热处理增强其结构稳定性,并以该多孔铜为基底电沉积获得三维多孔Cu6Sn5合金电极.采用循环伏安法研究了三维多孔Cu6Sn5合金电极的嵌/脱锂电位.采用电化学阻抗谱研究了三维多孔Cu6Sn5合金电极在不同温度下的首次嵌锂过程.结果显示,在主要的嵌锂区间内,三维多孔Cu6Sn5合...     

基于多孔硅的葡萄糖光学传感器

本实验通过对多孔硅硅表面涂敷一层智能凝胶~([1～3]),并在凝胶内包埋上葡萄糖氧化酶,使多孔硅.壳聚糖凝胶复合材料对葡萄糖分子产生体积溶胀响应,由于多孔硅及凝胶均对光有较好的反射性能,凝胶的溶胀过程产生Fabry-Perot薄膜反射干涉光谱的变化,将反射干涉光谱进行傅立叶变换后,可实时监测凝胶层薄膜的溶胀响应.     

Fabrication and characterization of porous Si-Al films anode with different macroporous substrates for lithium-ion batteries

Porous Si-Al films were fabricated by magnetron sputtering (co-sputtering) using three different copper substrates as current collectors, respectively. The morphology, compositions, structure, and crystallinity of the porous Si-Al films anodes were examined by using SEM, EDX, TEM, XRD, and Raman spectroscopy. The electrochemical properties of the porous Si-Al films anodes were evaluated by galvanostatic cycling. The Si-Al film deposited on copper foam showed higher insertion/extraction capacity, capacity retention, and longer cycle life in comparison to the Si-Al films deposited on expanded copper mesh and even copper mesh grid, which could be attributed to its unique three-dimensional macroporous structure. The three-dimensional macroporous structure could offer larger materials/electrolyte contact area, a much better adhesion, lower electrical resistance (i.e., well conductive), and stress-alleviated environment to partly accommodate volume expansion that leads to exfoliation during cycling.     

Novel Electroless Deposition of Cu<Subscript>3</Subscript>Se<Subscript>2</Subscript> Film on Silicon Substrate by a Simple Galvanic Displacement Process

A novel electroless deposition method for depositing highly uniform adhesive thin films of copper selenide (Cu₃Se₂) on silicon substrates from aqueous solutions is described. The deposition is carried out by two coupled galvanic reactions in a single deposition bath containing copper cations, hydrogen fluoride, and selenous acid: the galvanic deposition of copper on silicon and the subsequent galvanic reaction between the deposited copper with selenous acid in the deposition bath. The powder X-ray diffraction and scanning electron microscopy are used to characterize and examine the deposited films.     

Sol–Gel SiO2-ZrO2 Coatings for Optical Applications

SiO₂-ZrO₂ based nanostructured multilayers films have been prepared by sol–gel processing from metallorganic precursors by low temperature inorganic polymerization reactions. Simultaneous gelation of both precursors was realized. Homogeneous and transparent films were obtained at room temperature by dip- and spin-coating on glass and silicon wafer substrates. Samples with successively deposited layers (1–3 layers) and successive thermal treatments have been also studied. Each deposited layer was thermally treated for 1 h at 300°C. The coatings were characterized by XRD, spectroellipsometry (SE), UV-VIS spectroscopy and AFM methods. The influence of substrates, number of coatings and number of thermal treatments on the optical and structural properties of the films was established. The thickness of three deposited SiO₂-ZrO₂ layers is about 496 nm on glass substrates and 413 nm on the silicon wafer substrate. The films deposited on glass are more porous than those deposited on silicon. The properties of optical waveguide prepared from SiO₂-ZrO₂ layers on silicon substrates will be discussed.     

磁控溅射制备的铜钒氧化物薄膜及其电化学性能

采用射频磁控溅射技术在硅基底上分别制备了无掺杂和掺杂Cu的氧化钒薄膜. X射线衍射(XRD)分析和扫描电子显微镜(SEM)观察表明, 无掺杂的薄膜为多晶V2O5, 掺杂Cu的薄膜为非晶态. X射线光电子能谱(XPS)分析结果表明, 掺杂Cu的薄膜为铜钒氧化物膜, 其中Cu离子表现为+2价, V离子为+4与+5价的混合价态. 随着Cu掺杂量的增大, +4价V的含量增加. 电化学测试结果表明, V2O5薄膜在掺杂Cu以后其放电容量有显著的提高, 其中Cu2.1VO4.4薄膜在100次循环后容量还保持为83.4 μA·h·cm-2·μm-1, 表现出较高的放电容量和较好的循环性能.     

Preparation and investigation of nanostructured SnO2:Pd/ porous silicon/c-Si heterostructure solar cell

Journal of Solid State Electrochemistry - We have deposited pure SnO2 and SnO2:Pd nanostructure films on the quartz and porous silicon PSi substrates using chemical spray pyrolysis technique to...     

Solvothermal growth and morphology study of Cu2Se films

Solvothermal growth of cuprous selenide films on copper substrate has been succeeded by treating copper foil in the mixture of selenium powder and amines or hydrazine. The films were characterized by methods of XRD, SEM, TEM and optical spectra (Cu₂Se, JCPDS 47-1448). Films with hexagonal microcrystals can be obtained in hydrazine/water reaction system. When CTAB (CTAB = cetyltrimethylammonium bromide) is added to the system, the film is composed of thin leaf-like microcrystals. When ethylenediamine (en) is used as solvent, the leaf-like microcrystals are crimped.     

Matrix‐free laser desorption/ionization mass spectrometry using silicon glancing angle deposition (GLAD) films

Glancing angle deposition (GLAD) was used to fabricate nanostructured silicon (Si) thin films with highly controlled morphology for use in laser desorption/ionization mass spectrometry (DIOS‐MS). Peptides, drugs and metabolites in the mass range of 150–2500 Da were readily analyzed. The best performance was obtained with 500 nm thick films deposited at a deposition angle of 85°. Low background mass spectra and attomole detection limits were observed with DIOS‐MS for various peptides. Films used after three months of dry storage in ambient conditions produced mass spectra with negligible low‐mass noise following a 15 min UV‐ozone treatment. The performance of the Si GLAD films was as good as or better than that reported for electrochemically etched porous silicon and related materials, and was superior to matrix‐assisted laser desorption/ionization (MALDI)‐MS for analysis of mixtures of small molecules between 150–2500 Da in terms of background chemical noise, detection limits and spot‐to‐spot reproducibility. The spot‐to‐spot reproducibility of signal intensities (100 shots/spectrum) from 21 different Si GLAD film targets was ±13% relative standard deviation (RSD). The single shot‐to‐shot reproducibility of signals on a single target was ±19% RSD (n = 7), with no indication of sweet spots or mute spots. Copyright © 2010 John Wiley & Sons, Ltd.     

Synthesis of crystalline umangite phase of copper selenide (Cu3Se2) for TiO2 photoanode-based solar cell application

Journal of Solid State Electrochemistry - This study deals with the sensitization of the porous titanium oxide (TiO2) films deposited on fluorine doped tin oxide with copper selenide (Cu3Se2). The...     

XPS investigations of thin tantalum films on a silicon surface

Ultra thin tantalum-based diffusion barriers are of great interest in copper metallisation technology. Even the smallest amounts of copper that diffuse into the active silicon regions on a microprocessor will alter their semiconducting properties thus leading to failure of the device. In the present work Ta films were deposited on silicon by electron beam evaporation and magnetron sputtering. The background of this study is investigation of interface formation, which is expected to have substantial influence on the properties of thin Ta films. All experiments were carried out under UHV conditions. This was necessary because Ta is a very reactive metal and is readily oxidized even at low oxygen partial pressure. The Ta4f peak, as a sensitive indicator of the chemical state, was analysed and compared to that for standard samples. Silicide formation is assumed to occur at the Ta/Si interface.