X-ray diffractometry and electron microscopy of porous silicon layers at different stages of oxidation in air

Porous silicon layers prepared by anodic etching under different conditions have been systematically studied in the course of their natural oxidation (aging) in air by many-crystal X-ray diffractometry and transmission electron microscopy. Quantitative information on the strains and crystal structure of layers has been obtained using a combination of measurements of the 004 symmetric and 224 asymmetric reflections in the Bragg geometry on double-crystal and triple-crystal X-ray diffractometers. It has been revealed that the aging of porous silicon is accompanied by an increase in macrostrains and microstrains, as well as in micro-misorientations of crystal fragments, which lead to gradual destruction of porous layers up to their complete amorphization.     

The effect of oxidation on physical properties of porous silicon layers for optical applications

In order to understand the optical loss mechanisms in porous silicon based waveguides, structural and optical studies have been performed. Scanning and transmission electron microscopic observations of porous silicon layers are obtained before and after an oxidation process at high temperature in wet O₂. Pore size and shape of heavily p-type doped Si wafers are estimated and correlated to the optical properties of the material before and after oxidation. The refractive index was measured and compared to that determined by the Bruggeman model.     

Influence of experimental parameters on physical properties of porous silicon and oxidized porous silicon layers

This paper reports physical properties of porous silicon and oxidized porous silicon, manufactured by anodisation from heavily p-type doped silicon wafers as a function of experimental parameters. The growth rate and refractive index of the layers were studied at different applied current densities and glycerol concentrations in electrolyte. When the current density varied from 5 to 100 mA/cm², the refractive index was between 1.2 and 2.4 which corresponded to a porosity range from 42 to 85%. After oxidation, the porosity decreased and was between 2 and 45% for a refractive index range from 1.22 to 1.46. The thermal processing also induced an increase in thickness which was dependent on the initial porosity. This increase in thickness was more important for the lowest porosities. Lastly, the roughness of the porous layer/silicon substrate interface was studied at different applied current densities and glycerol concentrations in solution. Roughness decreased when the current density or glycerol concentration increased. Moreover, roughness was also reduced by thermal oxidation.     

用四探针及阳极氧化方法测量硅中扩散层杂质分布

本文讨论了:(1)用阳极氧化法在硅片表面去层的技术;(2)用四探针测量扩散层面电导的方法;(3)用阳极氧化去层及四探针测量面电导方法求得扩散层精细杂质分布。文中着重讨论了实验技术中的实际问题,如如何在阳极氧化过程中取得精细而均匀的去层(300—1500?);如何控制及测量去层厚度;测量面电导及杂质分布时的误差来源及减小误差的措施。以典型的磷在硅中扩散的杂质分布测量为例:扩散深度为4.9μm,测量间距为400—1600?,面电导测量误差估计小于3％,杂质分布误差估计小于20％。简单地提出了一些测量中尚待进一步解决的问题。     

氧化多孔硅/聚合物复合膜的折射率

用Bruggeman模型理论,分析了氧化多孔硅/聚合物复合膜的等效折射率与多孔硅孔隙率、氧化度和嵌入率的关系.实验研究了嵌入PMMA材料的氧化多孔硅/聚合物膜的等效折射率.证实了在多孔硅中嵌入聚合物可使薄膜的光学参量保持稳定.     

Stable ultraviolet photoluminescence emission in n-type porous silicon

This very paper is focusing on the investigation of porous silicon preparation with n-type silicon wafer by means of electrochemical anodization in the dark and, particularly, on its stable ultraviolet photoluminescence emission. A lateral electrical potential was applied, for this purpose, on silicon wafers, driving the electrons away and letting holes appear on the surface of the silicon wafer to enhance the electrochemical etching process. Characterizations have been made with scanning electronic microscope, fluorescence spectrophotometer and Fourier transform infrared spectroscope. An ultraviolet photoluminescence emission of 370 nm is found in the as-prepared n-type porous silicon, which seems to be well associated with the formation of oxygen-related species (twofold coordinated silicon defect) during the anodic oxidation. The result characterized by photo-bleaching performance indicates that the ultraviolet photoluminescence emission is so stable—only 7% reduction within 3600 s. Meanwhile the morphology of as-prepared n-type porous silicon is investigated.     

Infrared induced visible emission from porous silicon: the mechanism of anodic oxidation

The visible luminescence caused by anodic oxidation of p-type porous silicon has been studied. It is shown that similar luminescence can be observed in n-type material by illumination with near-infrared light. Addition of a suitable reducing agent to the electrolyte solution can both suppress the oxidation of the porous layer and quench its luminescence. These results confirm a previously suggested mechanism, in which the capture of a valence band hole in a surface bond of the porous semiconductor gives rise to a surface state intermediate capable of thermally injecting an electron into the conduction band.     

Simulation and fabrication study of porous silicon photonic crystal

The present work reports design and fabrication of porous silicon based one-dimensional (1D) photonic crystal. Distributed Bragg reflector (DBR) is a 1D photonic crystal composed of multilayer stack of high and low refractive index layers. Design of porous silicon DBR is a complex one and requires appropriate control in optical parameters of its constituent layers. In order to design DBR, two porous silicon single layer samples were fabricated using current density of 10 and 50 mA/cm². Optical characterization of single layer samples showed series of interference fringes. Reflective interferometric Fourier transform spectroscopy (RIFTS) method was employed to determine optical constants of porous silicon single layers. DBR simulation was carried out based on transfer matrix method. DBR was then fabricated using optical parameters obtained from RIFTS method. Reflection bandwidth of prepared DBR was found to be 216 nm, which is comparable to the simulated value of 203 nm.     

Discrete tunneling in electronic transport properties of nanograined porous silicon and similar heterophase systems

Experimental data obtained in the study of transverse current transport in a number of nanosized grained or similar media, such as porous silicon layers, anodic silicon oxide layers, and silicon nitride layers prepared by ion implantation of nitrogen into silicon, have been analyzed within the theory of discrete tunneling. It has been demonstrated that the measurements of current-voltage characteristics of diode structures with dielectric interlayers and embedded grains make it possible to obtain useful information on the character and sizes of grains or quantum dots in the nanosized grained medium. Amorphous dielectrics can be considered a grained medium with nanosized composition fluctuations. The current-voltage characteristics of real structures are determined by both the current nonlinearity associated with the charge carrier injection and the field nonlinearity caused by the Coulomb blockade of tunneling.     

Porous silicon bandgap broadening at natural oxidation

Emission and excitation photoluminescence spectra of porous silicon thin layers have been investigated at natural oxidation. The shift of both types of spectra to high-energy region with time has been shown. Analysis of excitation spectra points out the indirect behavior of electron transitions responsible for visible photoluminescence, which remains unaltered at natural oxidation. The value of optical bandgap is estimated in each case. It is shown that the optical bandgap broadens during oxidation due to size reduction of silicon nanocrystallites.     

Synthesis and characterization of porous silicon layers for 1D photonic crystal application

In this paper, we studied the optical and physical properties of electrochemically prepared porous silicon layers. The atomic force microscopy analysis showed that the etching depth, pore diameter and surface roughness increase as the etching time increased from 30 to 50 mA/cm². By tuning two current densities J₁ = 50 mA/cm² and J₂ = 30 mA/cm², two samples of 1D porous silicon photonic crystals were fabricated. The layered structure of 1D photonic crystals has been confirmed by scanning electron microscopy measurement which showed white and black strips of two distinct refractive index layers. Finally, the measured reflectance spectra of 1D porous silicon photonic crystals were compared with simulated results.     

Planar silicon-based light polarizers

Silicon-based thin-film polarizers operating in the visible and near-infraed spectral range are fabricated by electrochemical etching of bulk silicon wafers. Anisotropically etched (110) porous silicon layers exhibit a strong in-plane anisotropy of the refractive index. Stackes of alternating layers with different mean refractive indices and thicknesses act as dichroic Bragg reflectors or microcavities, respectively. Both structures have two distinct reflection and transmission bands depending on the polarization of the incident linearly polarized light. Planar polarizers are realized through the combination, in one structure, of a dichroic reflector with either a second reflector or a microcavity with different spectral responses.     

Luminescence and photosensitization properties of ensembles of silicon nanocrystals in terms of an exciton migration model

The relaxation processes that occur in ensembles of coupled silicon nanocrystals are described by a quantitative model that takes into account the energy transfer between them during exciton migration. This model is used to study the formation of singlet oxygen during the photoexcitation of silicon nanocrystals in porous silicon layers under various external conditions. It is experimentally found that, upon fine milling of as-deposited porous silicon films, the photoluminescence decay time increases despite an increase in the concentration of point defects. The photosensitized activity of ensembles of silicon nanocrystals degrades monotonically during their photostimulated oxidation. These experimental results agree completely with the conclusions of the model and are explained by a decrease in the number of exciton migration ways between nanocrystals when the granule size of a porous silicon powder decreases and by an increase in the efficiency of nonradiative recombination during the photostimulated oxidation of the nanocrystals. Our data indicate that nanocrystalline silicon is a promising material for the methods of nontoxic photodynamic therapy of oncological diseases.     

Confinement in a planar waveguide with porous silicon omnidirectional mirrors as confining walls

We present the design and study of waveguide structures based on porous silicon where the light confinement is not due to the usual total reflection effect but to the use of photonic crystals (PCs) as confining walls. These PC are omnidirectional mirrors (OMs), consisting of the periodic repetition of two porous silicon layers with different refractive indices and thicknesses. They reflect the radiation for all angles of incidence within a frequency range called the omnidirectional band gap (OBG). We have followed the PC formalism to investigate the properties of the OM as a multimode waveguide: the number of modes within the band gap, their field spatial distribution and their confinement as a function of the frequency and the core thickness.     

多孔硅薄层的正电子湮灭寿命研究

用阳极氧化法按不同腐蚀条件制备的多孔硅，其薄层厚度仅为几十纳米，远小于^22Na源的正电子平均射程．文章提出了一种用控Na的正电子测量体寿命谱并扣除基片贡献的方法，来确定多孔硅薄层的平均孔径。     

Determination of the effective refractive index of porous silicon/polymer composite films

The equation for calculating the effective refractive index of porous silicon inserted polymer was obtained by three-component Bruggeman effective medium model. The dependence of the effective refractive index of porous silicon/polymer composite films on the polymer fraction with various initial porosity was given theorically and experimentally respectively. The porous silicon and polymer polymethylmetacrylate based dispersive red one (PMMA/DR1) composite films were fabricated in our experiments. It is found that the measured effective refractive index of porous silicon inserted polymer was slightly lower than the calculated result because of the oxidization of porous silicon. The effective refractive index of oxidized porous silicon inserted polymer also was analyzed by four-component medium system.     

Surface layer reflective index changes of Au nanoparticle functionalized porous silicon microcavity for DNA detection

A technique is demonstrated to detect DNA hybridization based on surface layer of Au/porous silicon microcavity (Au/PSM) substrate for very small amount of biomolecules. Simulations show that the increase of effective refractive index for the first layer of PSM will cause a blue shift for its reflectance spectrum, and the blue shift becomes less with the increase of refractive index for one more layers. In experiments, such a blue shift of reflectance spectrum of PSM comes from the increase of refractive index by DNA hybridization on the surface. The detection limit of Au/PSM biosensor is 15.15 nM for 19-base pair DNA, which is comparable to that of reported biosensors based on porous silicon (PS). Therefore such an Au/PSM could be very useful to develop simple, rapid and sensitive optical biosensors when the amount of target is very small.     

Silicon microlens structures fabricated by scanning-probe gray-scale oxidation

We report on the micromachining of silicon microlens structures by use of scanning-probe gray-scale anodic oxidation along with dry anisotropic etching. Convex, concave, and arbitrarily shaped silicon microlenses with diameters as small as 2 microm are demonstrated. We also confirm the high fidelity of pattern transfer between the probe-induced oxides and the etched silicon microlens structures. Besides the flexibility, the important features of scanning-probe gray-scale anodic oxidation are small pixel size and pitch (of the order of tens of nanometers), an unlimited number of gray-scale levels, and the possibility of creating arbitrarily designed microlens structures with exquisite precision and resolution. With this approach, refractive, diffractive, and hybrid microlens arrays can be developed to create innovative optical components.     

Realisation of a humidity sensor based on perfect metamaterial absorber

In this paper, we have proposed and investigated a humidity sensor based on perfect metamaterial absorber. The sensor is composed of three layers, which are metallic particle array on the top, porous silicon in the middle layer and metallic film at the bottom. According to the effective medium approximation, the effective permittivity of porous silicon is mainly determined by the filling fraction of water condensation. It is shown that the resonant wavelength displays significant red-shift with the increasing effective permittivity of porous silicon. Furthermore, the simulation results indicate that the refractive index sensitivity of absorber is high to 249 nm/RIU, which makes our structure be an ideal candidate for evaluating the humidity of environment.     

多孔硅光致发光峰半峰全宽的压缩

硅发光对于在单一硅片上实现光电集成是至关重要的.目前已有的使硅产生发光的方法有:掺杂深能级杂质、掺稀土离子、多孔硅、纳米硅以及Si/SiO₂超晶格.声空化所引发的特殊的物理、化学环境为制备光致发光多孔硅薄膜提供了一条重要的途径.实验表明,声化学处理对于改善多孔硅的微结构,提高发光效率和发光稳定性都是一项非常有效的技术.超声波加强阳极电化学腐蚀制备发光多孔硅薄膜,比目前通用的常规方法制备的样品显示出更优良的性质.这种超声波的化学效应源于声空化,即腐蚀液中气泡的形成、生长和急剧崩溃.在多孔硅的腐蚀过程中,由于超声波的作用增加了孔中氢气泡的逸出比率和塌缩,有利于孔沿垂直方向的腐蚀,使多孔硅光致发光峰的半峰全宽压缩到了3.8nm.