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。     

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．     

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．     

多孔玻璃制备及其与Al2O3陶瓷基板复合载体材料

在钠硼硅玻璃体系中利用分相原理制备得到纳米多孔玻璃,并运用SEM、BET测试手段表征了纳米多孔玻璃的孔径分布、孔径大小和比表面积,以及热处理温度和时间对多孔玻璃表面形貌的影响.通过对纳米孔玻璃与氧化铝陶瓷基片复合的研究,得到一种能贮存大量生物和化学样本的载体材料,对生物芯片的发展将起到推动作用.     

多孔玻璃制备及其与A12O3陶瓷基板复合载体材料

在钠硼硅玻璃体系中利用分相原理制备得到纳米多孔玻璃,并运用SEM、BET测试手段表征了纳米多孔玻璃的孔径分布、孔径大小和比表面积,以及热处理温度和时间对多孔玻璃表面形貌的影响。通过对纳米孔玻璃与氧化铝陶瓷基片复合的研究,得到一种能贮存大量生物和化学样本的载体材料,对生物芯片的发展将起到推动作用。     

多孔硅表面氧化钒热敏电阻薄膜的阻温特性

用电化学腐蚀法制备了具有不同导热系数的多孔硅样品(孔隙率为80％±2、厚度为110μm时,导热系数可降低至0．20 W／m·K),并在其表面沉积了氧化钒热敏薄膜,研究了多孔硅样品的热绝缘性能对氧化钒热敏薄膜阻温特性的影响．结果表明:多孔硅良好的热绝缘性使在其表面制备的氧化钒热敏薄膜电阻的灵敏度远高于在硅基底上制备的热敏电阻的(多孔硅和硅片上的氧化钒薄膜电阻随功率变化斜率分别为120 kΩ／μW和2．1 kΩ／μW),且热敏电阻的灵敏度随着多孔硅孔隙率和厚度的增大而升高．     

电偶腐蚀法制备多孔硅的研究EI

用电偶腐蚀法制备多孔硅,主要研究了铂电极的优化制备工艺以及腐蚀条件对多孔硅厚度的影响,并且结合SEM,AFM等测试手段对所制备的多孔硅的表面形貌进行了分析。实验发现,在相同的腐蚀条件下,多孔硅的厚度随铂电极的厚度以及铂电极与腐蚀硅片的面积比的增大而增大。     

多孔硅基热敏薄膜的制备与性能

对MEMS用具有绝热性能的多孔硅基底上沉积的热敏感薄膜进行了研究．首先用电化学方法制备多孔硅,分别在多孔硅基底和硅基底上通过溅射镀膜方法沉积氧化钒、Cu、Au热敏薄膜,测试多孔硅基底和硅基底上的氧化钒及金属薄膜电阻的热敏特性．结果表明,在多孔硅基底表面沉积的热敏薄膜具有与硅基表面热敏薄膜同样的热敏特性且表现出更高的灵敏度;此外,对沉积在不同制备条件得到的多孔硅上的氧化钒薄膜电阻热敏特性进行比较,发现随着孔隙率和厚度的增加,多孔硅的绝热性能提高,其上沉积的氧化钒薄膜电阻热敏特性增强．     

多孔玻璃粉的制备及其在玻璃基板上的粘接

利用硼硅酸盐玻璃的分相和酸侵蚀制备了孔径可控的多孔玻璃粉,采用SEM、BET等测试手段对玻璃的表面形貌和孔径分布进行了表征。并以Na2O-Al2O3-B2O3体系低熔点玻璃作为粘接剂将多孔玻璃粉烧结在普通玻璃板上,研制出一种表面孔径约50nm且均匀分布的多孔玻璃基板,并分析了烧结温度、烧结时间、颗粒大小等对粘接的影响。     

多孔硅在高温退火过程中结构变化的研究

采用电化学腐蚀的方法制备了不同孔径的多孔硅薄膜样品,并在1050℃高温下进行了退火。采用扫描电镜和拉曼光谱对多孔硅退火前后结构的变化进行了观察,根据晶体形核理论分析了孔径变化的机理,并从热力学角度对其微观机制进行了讨论。实验和理论分析的结果均表明,多孔硅的初始孔径存在一个临界值,初始孔径小于此临界值时,孔在高温退火中有收缩的趋势;反之,初始孔径大于此临界值时,孔有变大的趋势。     

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。     

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。     

Porous silicon as a versatile platform for laser desorption/ionization mass spectrometry

Desorption/ionization on porous silicon mass spectrometry (DIOS-MS) is a novel method for generating and analyzing gas-phase ions that employs direct laser vaporization. The structure and physicochemical properties of the porous silicon surfaces are crucial to DIOS-MS performance and are controlled by the selection of silicon and the electrochemical etching conditions. Porous silicon generation and DIOS signals were examined as a function of silicon crystal orientation, resistivity, etching solution, etching current density, etching time, and irradiation. Pre-and postetching conditions were also examined for their effect on DIOS signal as were chemical modifications to examine stability with respect to surface oxidation. Pore size and other physical characteristics were examined by scanning electron microscopy and Fourier transform infrared spectroscopy, and correlated with DIOS-MS signal. Porous silicon surfaces optimized for DIOS response were examined for their applicability to quantitative analysis, organic reaction monitoring, post-source decay mass spectrometry, and chromatography.     

Fabrication of a porous polyimide membrane using a silicon nanowire array as a template

We demonstrate that a porous polyimide membrane can be fabricated by curing liquid polyimide on a vertically oriented silicon nanowire array and selectively etching away the nanowire-array-template using xenon difluoride (XeF₂). Pore size and density using the described technique are controllable. The former is dependent on nanowire diameter and the duration of etching, whereas pore density is determined by silicon nanowire density. We believe that the described porous membrane fabrication method can be applied to various polymer and nanowire systems.     

Blue luminescence from porous layers produced by metal-assisted chemical etching on low-doped silicon

Photoluminescent porous layers were formed on highly resistive p-type silicon by a metal-assisted chemical etching method using K₂Cr₂O₇ as an oxidizing agent. A thin layer of Ag is deposited on the (1 0 0) Si surface prior to immersion in a solution of HF and K₂Cr₂O₇. The morphology of the porous silicon (PS) layer formed by this method as a function of etching time was investigated by scanning electron microscopy (SEM). It shows that the surface is formed by macropores filled with microporous silicon. The porous layers were characterized by backscattering spectrometry (BS) as a function of etching time in random and channelling mode. Channelling spectra show that the porous layer remains crystalline after etching. On the other hand, random and channelling spectra show that the deposited silver diffuses into the pore. Luminescence from metal-assisted chemically etched layers was measured. It was found that the PL intensity increases with increasing etching time. This behaviour is attributed to increase of the density of the silicon nanostructure. Finally, the PL spectra show two peaks of emission at 450 and 600 nm.     

阳极氧化电流密度和时间对多孔硅形貌和电子发射特性的影响

为了应用于场发射显示器,采用电化学阳极氧化,快速热氧化和磁控溅射等方法制备出了金属/多孔硅/硅基底/金属结构的多孔硅电子发射体,并运用扫描电子显微镜观察了多孔硅的微观形貌,结果发现多孔硅的孔径随着电化学阳极氧化电流密度的增加而增加,多孔硅层的厚度随着阳极氧化电流密度和时间乘积的增加而增加。在真空系统中测量了多孔硅的电子发射特性,电子发射的阈值电压Vth随着多孔硅层厚度的增加而增加;最大的发射效率η为7.5‰,此效率出现在孔径6~16 nm,多孔硅层厚度为11.06μm的样品中,对应的器件电压Vps为30V。     

Study of anodization parameters effects on photoconductivity of porous silicon

We have prepared porous silicon by etching p-type crystalline silicon in different conditions such as: varying electrolyte concentration, current density, and etching time. The primary objective of this research is to develop a scientifically based technique for the measurement of photosensitivity. One such technique involves measuring the photoconductivity of the porous silicon under halogen lamp irradiation. Our photoconductivity measurements agree with photoluminescence measurements in previous work, and demonstrate the direct transition of porous silicon. Varied etching conditions change the peak of photoconductivity from 600 to 520 nm (from 2.13 eV to 2.4 eV) as the porosity of the layer gradually increases, and the photoconductivity band also becomes slightly more intense. The photoconductivity peak shift toward shorter wavelength was interpreted to be the result of band gap widening. We observe two distinct regimes in the time decay of photoconductivity, fast decay and steady state, that arise from the recombination process and electron–hole asymmetry near the Fermi surface. Experimental measurements of photoconductivity give useful information about the band gap, band structure, and variation of transport properties due to the micro-structural porosity created during the etching process.     

电催化金属辅助化学刻蚀法制备硅纳米线/多孔硅复合结构

量子限制效应使硅纳米线具有良好的场致发射特性, 结合多孔硅的准弹道电子漂移模型可提高场发射器件的性能。传统的金属辅助化学刻蚀法制备硅纳米线的效率较低, 本研究在传统方法的基础上引入恒流源, 提出电催化金属辅助化学刻蚀法, 高效制备了硅纳米线/多孔硅复合结构。在外加30 mA恒定电流的条件下, 硅纳米线的平均制备速率可达308 nm/min, 较传统方法提升了173%。研究了AgNO₃浓度、刻蚀时间和刻蚀电流对复合结构形貌的影响规律; 测试了采用电催化金属辅助化学刻蚀法制备样品的场发射特性。结果显示样品的阈值场强为10.83 V/μm, 当场强为14.16 V/μm时, 电流密度为64 μA/cm²。     

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.     

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。