采用原电池法制备纳米多孔硅

利用原电池法在硅片表面制备了纳米多孔硅层;用扫描电镜SEM和原子力显微镜AFM观察了多孔硅表面形貌：原电池法与电化学法得到的多孔硅孔径均在10～20nm范围．研究结果表明：铂膜电极厚度的增大以及铂膜电极与暴露硅片面积比的增大,会导致多孔硅层的厚度增大．热学模拟结果表明：以纳米多孔硅作为绝热层可获得与悬浮结构相同的效果．     

纳米多孔硅的电化学制备及性能研究

纳米多孔硅是一种潜在的化学和生物传感材料,本文采用电化学腐蚀法制备纳米多孔硅。采用SEM技术分析多孔硅的表面形貌,研究了腐蚀条件对多孔硅的孔隙率、厚度、I-V特性的影响。结果表明,多孔硅的孔隙率随着腐蚀电流密度和腐蚀时间的增加而呈线性增大趋势;其厚度随着腐蚀电流密度的增加而近似呈线性增大趋势,随腐蚀时间的成倍增加而显著增大;其I-V特性表现出非整流的欧姆接触。     

多孔硅的电化学制备与研究

以电化学方法制备了多孔硅材料并通过表面轮廓测试仪、原子力显微镜、显微拉曼光谱仪等设备对制备多孔硅的孔隙率、厚度、表面形貌、以及热导率进行了表征.结果发现,本实验制备的多孔硅属于介孔硅(15～20nm),其孔隙率随腐蚀时间和腐蚀电流的变化有先增大后减小的趋势.增加多孔硅的厚度和孔隙率,可以使得多孔硅的热导率显著降低(最低可低至0.62W/m·K).     

电化学腐蚀多孔硅表面形貌的结构特性

多孔硅作为微电子机械系统中重要的热绝缘层和牺牲层材料,其表面形貌结构特性是影响多孔硅上薄膜器件性能的重要因素,为此,利用双槽电化学腐蚀方法制备了多孔硅薄膜,并通过原子力显微镜和场发射扫描电子显微镜对制备多孔硅的表面形貌和孔径大小分布进行了观察．结果发现：腐蚀初期,在硅表面会有大量的硅柱形成,硅柱的直径、高度、分布密度与电流密度成正比关系;硅柱在进一步腐蚀过程中会消失,多孔硅的表面粗糙度随着腐蚀的进行,先减小再增大,最后达到稳定值0．52nm;多孔硅孔径大小分布区间随腐蚀时间增加变窄．     

直流电化学腐蚀法制备多孔硅的表面形貌研究

采用正交实验，直流电化学腐蚀法制备多孔硅。用原子力显微镜对表面进行观察，研究电化学腐蚀参数对其表面形貌的影响。氢氟酸浓度（CHF）升高，使临界电流密度（JPS）增大，有利于多孔硅的形成。电流密度（J）增大，多孔硅的孔隙率和孔径随之变大，而其纳米粒径将变小。腐蚀时间（t）越长，孔径越大，孔越深。     

多孔硅对单晶硅少子寿命影响状况的研究

以p型单晶硅片为研究对象,在单晶硅片表面采用化学腐蚀方法制备多孔硅层,通过实验选取制备多孔硅的最佳工艺条件,采用SEM观察多孔硅表面形貌,以及用微波光电导法测试少子寿命的变化情况。结果表明,在相同的腐蚀溶液配比条件下腐蚀11min得到的多孔硅层的表面形貌最好,孔隙率最大。在850℃下热处理150min时样品少子寿命的提高达到最大,不同腐蚀时间的样品少子寿命提高程度不同,腐蚀11min的样品少子寿命提高最大,约有10%左右。多孔层的形成伴随着弹性机械应力的出现,引起多孔层-硅基底界面处产生弹性变形,这有利于缺陷和金属杂质在界面处富集。另外,多孔硅仍具有晶体结构,但其表面方向上的晶格参数要比初始硅的晶格参数大,也有利于金属杂质向多孔层迁移。     

应用于微电子机械系统中多孔硅的研究

针对多孔硅在MEMS中作为牺牲层和绝热层的应用,主要研究了电化学腐蚀法制备多孔硅的实验条件与多孔硅深度及其孔隙率间的关系,实验发现电化学腐蚀法制备多孔硅的腐蚀速率在腐蚀前期阶段基本是一定值(电流密度为80mA/cm2时为1.3μm/min,电流密度为40 mA/cm2时为0.4μm/min),但到腐蚀后期阶段随着孔深的增加有所下降.同时发现对于不同的腐蚀电流密度,多孔硅的孔隙率都有随腐蚀时间的延长先增加后降低的趋势,用Beale模型可以很好的解释这一现象.最后,针对多孔硅在制备后易发生龟裂的现象,用拉曼光谱分析了多孔硅的内部应力情况,结果表明随多孔硅孔隙率的上升其内部残余应力有增加的趋势.     

MEMS中多孔硅绝热技术

主要介绍了多孔硅的制备方法(化学法、电化学法及原电池法等)、多孔硅导热系数测试的几种常用手段(温度传感器法、显微拉曼散射法及光声法等)、导热系数的理论模型及影响因素．此外,采用不同方法制备了多孔硅样品,分析了其表面形貌并用显微拉曼光谱法测定了导热系数．结果发现,化学法制备的多孔硅孔径尺寸大于微米量级,而利用大孔硅电化学和原电池法得到的样品孔径尺寸小(约20nm),属于介孔硅．由于腐蚀条件的不同,多孔硅的孔隙率和厚度也不同,多孔硅的导热系数随孔隙率和厚度的增大而迅速减小．     

多孔硅层孔隙率对其热绝缘性能的影响

研究了多孔硅层孔隙率对其热绝缘性能的影响机制.以P 型硅片为基底,通过双槽电化学腐蚀法制备多孔硅.采用微拉曼光谱法对多孔硅的热导系数进行了测量,结果表明,多孔硅的热导系数随其孔隙率的增大而明显下降,实验中热导系数最低可达到0.624W/(m·K),从而通过降低热导系数使多孔硅的绝热性能得到了增强.     

多孔硅的制备及其吸杂处理对电学性能的影响

多孔硅吸杂是减少晶体硅中杂质和缺陷,提高太阳能电池转换效率的有效方法。采用电化学腐蚀方法在单晶硅片上制备多孔硅,通过观察多孔硅的形貌、结构及单晶硅片的电阻率变化,研究不同电流密度制备的多孔硅对吸杂效果的影响,并从多孔硅的结构出发探究多孔硅吸杂的机理。结果表明,随电流密度增加,孔隙率明显增加,多孔硅在电流密度为100mA/cm2时,孔隙率最大;电流密度越大,多孔硅伴随所产生的弹性机械应力增加,晶格常数相应增加,这两个因素都有利于缺陷和金属杂质在多孔硅层-基底界面处迁移和富集,导致单晶硅吸杂后电阻率增大。     

Multi-spot porous silicon chip prepared from asymmetric electrochemical etching for human immunoglobin G sensor

Multi-spot porous silicon (MSPS)-based optical biosensor was developed to specify the biomolecules. MSPS chip was generated by an electrochemical etching of silicon wafer using an asymmetric electrode configuration in aqueous ethanolic HF solution and constituted with nine arrayed porous silicon. MSPS prepared from anisotropic etching conditions displayed the Fabry-Pérot fringe patterns which varied spatially across the porous silicon (PS). Each spot displayed different reflection resonances and different pore characteristics as a function of the lateral distance from the Pt counter electrode. The sensor system consists of the 3 x 3 spot array of porous silicon modified with Protein A. The system was probed with various fragments of an aqueous Human Immunoglobin G (Ig G) analyte. The sensor operated by measurement of the reflection patterns in the white light reflection spectrum of MSPS. Molecular binding and specificity was detected as a shift in wavelength of these Fabry-Pérot fringe patterns.     

Photochemical wet etching of silicon by synchrotron white X-ray radiation

We have investigated photochemical wet etching of n-type silicon (100) using synchrotron white X-ray radiation. During electroless photochemical wet etching under high flux white X-ray beam, the surface is electropolished. However, when the photon is reduced, the silicon surface becomes porous instead. The pore formation is greatly enhanced when an external potential is applied through a Pt counter electrode. The porous silicon layer exhibits strong photoluminescence signal.     

Controllable and Facile Fabrication of Gold Nanostructures for Selective Metal‐Assisted Etching of Silicon

A method with the combination of organic‐vapor‐assisted polymer swelling and nanotransfer printing (nTP) is used to manufacture desirable patterns consisting of gold nano‐clusters on silicon wafers for Au‐assisted etching of silicon. This method remarkably benefits to the size control and regional selection of the deposited Au. By tuning the thickness of the Au films deposited on the polydimethylsiloxane (PDMS) stamps, along with the swelling of PDMS stamps in acetone atmosphere, the Au films are cracked into diverse nanostructures. These nanostructures are covalently transferred onto silicon substrates in a large scale and enable to accelerate the chemical etching of silicon. The etched areas are composed of porous structures which can be readily distinguished from the surroundings on optical microscope. PDMS stamps and the Au clusters provide the control over the feature of the etched areas and the porous silicon, respectively. The silicon surfaces with patterned porous features offer a platform for exploiting new functional templates, for example, they present a diversity of antireflective and fluorescent performance.     

多孔硅的微结构及其冷阴极的电子发射特性研究

采用电化学腐蚀法在n型单晶Si基底上制备多孔硅(PS)膜,利用场发射扫描电子显微镜(FE-SEM)分析其微结构特征,研究了硅基底材料、腐蚀电流密度和腐蚀时间等制备条件和工艺参数对PS微结构的影响。实验结果表明,轻掺杂n型Si基底上形成的PS膜(n--PS)中的孔较深且孔径较大,而重掺杂n型Si基底上的PS膜(n+-PS)中的孔分布较为密集,而且呈多分枝结构;腐蚀电流密度相同时,PS的膜厚和腐蚀时间成正比,而在较高的腐蚀电流密度下制备得到的PS膜在结构上更为疏松。制作了基于n+型硅基底的PS阴极,此阴极的阈值电压约为14 V,高于该电压后发射电流随着二极管电压提高而呈指数性增加趋势,而且发射电流对环境气压不敏感,即使在0.1 Pa的低真空中也没有明显的衰减。     

Step voltage with periodic hold-up etching: A novel porous silicon formation

A novel etching method for preparing light-emitting porous silicon (PS) is developed. A gradient steps (staircase) voltage is applied and hold-up for different periods of time between p-type silicon wafers and a graphite electrode in HF based solutions periodically. The single applied staircase voltage (0–30 V) is ramped in equal steps of 0.5 V for 6 s, and hold at 30 V for 30 s at a current of 6 mA. The current during hold-up time (0 V) was less than 10 μA. The room temperature photoluminescence (PL) behavior of the PS samples as a function of etching parameters has been investigated. The intensity of PL peak is initially increased and blue shifted on increasing etching time, but decreased after prolonged time. These are correlated with the study of changes in surface morphology using atomic force microscope (AFM), porosity and electrical conductance measurements. The time of holding-up the applied voltage during the formation process is found to highly affect the PS properties. On increasing the holding-up time, the intensity of PL peak is increased and blue shifted. The contribution of holding-up the applied steps during the formation process of PS is seen to be more or less similar to the post chemical etching process. It is demonstrated that this method can yield a porous silicon layer with stronger photoluminescence intensity and blue shifted than the porous silicon layer prepared by DC etching.     

化学刻蚀法制备多孔硅的表面形貌研究

应用各种表面形貌分析方法如SEM、TEM、AFM等,通过对用化学刻蚀法形成的多孔硅进行表面形貌分析,发现由于横向腐蚀比较严重而使多孔硅层在达到一定深度后就会自动脱落。腐蚀中由于大量H2的析出,对硅晶体产生巨大的应力,这些应力使硅在比较脆弱的晶粒边界或缺陷处产生微裂纹,多孔硅就从这些地方开始和生长。     

Fabrication of gradient optical filter containing anisotropic Bragg nanostructure

New gradient optical filters containing asymmetric Bragg structure were prepared from the distributed Bragg reflector (DBR) porous silicon (PSi). Anisotropic DBR PSi displaying a rainbow-colored reflection was generated by using an asymmetric etching configuration. Flexible anisotropic DBR PSi composite films were obtained by casting of polymer solution onto anisotropic DBR PSi thin films. The surface and cross-sectional images images of anisotropic DBR PSi composite films obtained with cold field emission scanning electron microscope indicated that the average pore size and the thickness of porous layer decreased as the lateral distance increased. As lateral distance increased, the reflection resonance shifted to shorter wavelength.     

多孔硅-酶复合电极对葡萄糖溶液的电化学检测

多孔硅（PS）具有纳米级尺寸,高的表面积比和生物兼容性为固定生物分子提供了有利的条件。文章采用光电化学腐蚀的方法制备出多孔硅,并将3-氨基丙基三乙氧基硅烷（APTS）共价结合到多孔硅表面实现其生物功能化。通过戊二醛（Gluta）交联的方式将葡萄糖氧化酶（GOD）固定到生物功能化多孔硅上,形成GOD-Gluta-APTS-PS复合结构并用作电化学测量的工作电极。铂金和饱和甘汞电极分别作辅助电极和参比电极。通过测量还原电流对数与电极电势的关系以及计时电流曲线,对10×10^-6-55×10^-6mol dm^-3浓度范围的葡萄糖水溶液进行测量分析,发现还原电流与葡萄糖溶液在一定范围内有线性响应关系。制成的多孔硅酶复合电极间隔5天重复使用1次,20天内性能能保持基本不变。