Morphology and distribution of subsurface damage in optical fused silica parts: Bound-abrasive grinding

The depth and morphology of subsurface damage (SSD) in fused silica samples ground with diamond grinding wheels were investigated. The factors possibly influencing the SSD depth of ground samples were examined. The results demonstrate that the SSD depth is most responsive to diamond grit size while the processing parameters (i.e. depth of cut, feed rate, and wheel peripheral speed) have marginal effects on the SSD depth. The SSD depth decreases with the abrasive/grit size of diamond wheels and slightly diminishes with the decrease of cutting depth but little influenced by feeding rate and wheel speed. The morphology inspection shows that the density of subsurface cracks in ground fused silica samples decays exponentially with the depth from the ground surface into the bulk and the cracks vanish at a certain depth that depends on the mechanical and physical properties of samples and diamond abrasives/grits.     

Characterization of porous silicon prepared by powder technology

In this study, we have proposed the powder technology as new method for preparation of bulk porous silicon. Formation of porous silicon by high-energy ball milling followed by pressing and sintering was studied by X-ray diffraction, scanning electron microscopy and X-ray photoelectron spectroscopy (XPS). A crystalline wafer with (1 1 1) orientation was extensively ball milled up to 72 h leading to a decrease in average crystallite size up to 15 nm. The most significant reduction of crystallite size was observed after milling process for about 24 h. The nanopowders were then pressed into pellets at a pressure up to 400 MPa and sintered at 1173 K for 60 min in a high purity argon atmosphere. Results showed that after sintering the material became porous with uniform porosity in whole volume, independently of the sinter size. It is not possible to prepare such porous materials using the conventional electrochemical etching, where the porous structure depth usually does not exceed tens of micrometers. Core-level XPS studies showed very good agreement between peak positions of the sintered porous silicon and in-situ prepared polycrystalline 20 nm-Si thin film or single-crystalline Si (1 1 1) wafer. Furthermore, the valence band spectra measured for sintered samples are broader compared to those measured for the Si (1 1 1) wafer or polycrystalline Si thin film. On the other hand, the shape and broadening of the valence bands measured for the sintered samples are in very good agreement with those reported for electrochemically prepared porous silicon.     

Material removal effect of microchannel processing by femtosecond laser

Material processing using ultra-short-pulse laser is widely used in the field of micromachining, especially for the precision processing of hard and brittle materials. This paper reports a theoretical and experimental study of the ablation characteristics of a silicon wafer under micromachining using a femtosecond laser. The ablation morphology of the silicon wafer surface is surveyed by a detection test with an optical microscope. First, according to the relationship between the diameter of the ablation holes and the incident laser power, the ablation threshold of the silicon wafer is found to be 0.227 J/cm². Second, the influence of various laser parameters on the size of the ablation microstructure is studied and the ablation morphology is analyzed. Furthermore, a mathematical model is proposed that can calculate the ablation depth per time for a given laser fluence and scanning velocity. Finally, a microchannel milling test is carried out on the micromachining center. The effectiveness and accuracy of the proposed models are verified by comparing the estimated depth to the actual measured results.     

TEM and photoluminescence characterization of porous-silicon layers from <111>-oriented p + silicon substrates

Summary A first structural investigation, carried out by transmission electron microscopy on porous-silicon samples fromp ⁺, <111>-oriented substrates is presented. The samples, which show intense visible room temperature luminescence, are composed by an interconnected network of crystalline nanostructures. Evidences of the pores propagation along the <100> directions are provided. The optical and morphological characteristics of the investigated samples are found to be much similar to those of samples coming fromp-type, non-degenerate, <100>-oriented substrates rather than those obtained from <100> substrates with comparable resistivity. This striking effect is explained by invoking different etch-limiting mechanisms during pore formation. Their relative weights are proposed to depend on the crystallographic orientation of the silicon specimen subjected to etching. Paper presented at the III INSEL (Incontro Nazionale sul Silicio Emettitore di Luce), Torino, 12–13 October 1995.     

平面光学元件研磨抛光磨粒运动轨迹曲率研究

为提高研磨抛光加工表面质量,利用Matlab软件编制程序对不同参数下轨迹曲线曲率进行计算分析。结果表明,转速比对磨粒运动轨迹曲线曲率影响很大;相同转速比下的曲线曲率呈现周期性变化,曲率变化幅值很小;磨粒径向距离越大,曲率变化越剧烈,工件边缘处容易产生曲率突变;考虑到对磨粒径向距离的影响,偏心距不宜太大或太小。同时,磨粒初始角度对磨粒轨迹曲线曲率形状没有影响。该研究可为研磨抛光设备的设计提供理论指导。     

Experimental investigation on laser-induced surface damage threshold of Nd-doped phosphate glass

Nd-doped phosphate glass is the dominant amplifier material used in solid state high average power laser systems.Surface imperfection and subsurface damage(SSD)of the glass,resulting from the optical fabrica-tion process,limit the increment of laser system energy output.Thus,it is important to enhance the surface damage threshold of Nd-doped phosphate glass surface.The influence of abrasive size,polishing powder,grinding mode,and chemical treatment on the laser-induced damage threshold(LIDT)of Nd-doped phos-phate glass surface is investigated.Results show that the LIDT is affected little by different polishing powders and grinding modes.The LIDT correlates with the abrasive size,which produced different depths of SSD.A suitable acid etching treatment can remove the imperfection and the SSD for improving the LIDT of Nd-doped phosphate glass surface.The combination of several effective techniques and methods,which are low-cost and practical,should be useful to enhance the LIDT of Nd-doped phosphate glass surface.     

Surface disorder in c-Si induced by swift heavy ions

The disorders induced in crystalline silicon (c-Si) through the process of electronic energy loss in the swift heavy ion irradiation were investigated. A number of silicon <1 0 0> samples were irradiated with 65 MeV oxygen ions at different fluences, 1×10¹³ to 1.5×10¹⁴ ions/cm², and characterized by the Raman spectroscopy, the optical reflectivity, the X-ray reflectivity, the atomic force microscopy (AFM) and the X-ray diffraction (XRD) techniques. The intensity, redshift, phonon coherence length and asymmetric broadening associated with the Raman peaks reveal that stressed and disordered lattice zones are produced in the surface region of the irradiated silicon. The average crystallite size, obtained by analyzing Raman spectrum with the phonon confinement model, was very large in the virgin silicon but decreased to<100 nm dimension in the ion irradiated silicon. The results of the X-ray reflectivity, AFM and optical reflectivity of 200–700 nm radiation indicate that the roughness of the silicon surface has enhanced substantially after ion irradiation. The diffusion of oxygen in silicon surface during ion irradiation is evident from the oscillation in the X-ray reflectivity spectrum and the sharp decrease in the reflectivity of 200–400 nm radiation. The rise in temperature, estimated from the heat spike model, was high enough to melt the local silicon surface. The results of XRD indicate that lattice defects have been induced and a new plane <2 1 1> has been formed in the silicon <1 0 0>after ion irradiation. The results of the present study show that the energy deposited in crystalline silicon through the process of electronic energy loss ～0.944 keV/nm per ion is sufficient to induce disorders of appreciable magnitude in the silicon surface even at a fluence of ～10¹³ ions/cm².     

Controlling subsurface damage in neodymium-doped phosphate glass

We investigate the removal mechanism of neodymium-doped phosphate glass dominated in loose abrasive grinding and bound abrasive grinding. Moreover, we investigate the surface roughness and subsurface damage change with optical fabrication parameters, such as different spindle speed, load and abrasive size under different grinding processes in details. For a range of experimental conditions, we find that fracture is the principal removal mechanism for loose abrasive grinding, while plastic scratching is the dominating mechanism for bound abrasive grinding. The load has more influence on subsurface damage for bound abrasive grinding than for loose abrasive grinding. However, the spindle speed has different effect on subsurface damage produced with loose abrasive grinding and bound abrasive grinding. Moderate spindle speed and low load is preferred to produce smaller subsurface damage for loose abrasive grinding. Moreover, higher spindle speed and lower load are preferred to plastic scratching for bound abrasive grinding. Bound abrasive grinding produces 4 times lower surface roughness and 3 times lower subsurface damage than loose abrasive grinding.     

Mechanism of light emission in low energy ion implanted silicon

A silicon wafer implanted with a single low energy (42 keV) silicon ion beam results in strong luminescence at room temperature. The implantation results in the formation of various luminescent defect centers within the crystalline and polymorphous regions of the wafer. The resulting luminescence centers (LC) are mapped using fluorescence lifetime imaging microscopy (FLIM). The emission from the ion-implanted wafer shows multiple PL peaks ranging from the UV to the visible; these emissions originate from bound excitonic states in crystal defects and interfacial states between crystalline/amorphous silicon and impurities within the wafer. The LCs are created from defects and impurities within the wafer and not from nanoparticles.     

脆性光学材料的超声磨削实验研究

分别采用超声磨削和普通磨削加工方法加工了几种脆性光学材料,研究了几种主要工艺参数对工件加工表面粗糙度的影响。结果表明,超声频率和振幅、金刚石磨料粒度、切深、工具的横向进给速度和旋转速度等工艺参数对表面粗糙度的影响较大。通过比较发现,超声磨削方法比普通磨削方法具有更好的加工表面粗糙度,更高的材料去除率,以及更低的工具磨损量。     

Comparative experimental study of laser-induced transitions in crystalline silicon by femtosecond,picosecond, and millisecond laser ablation

In order to study laser-induced transitions of the crystalline silicon, comparative ablation experiments by femtosecond-, picosecond-, and millisecond-pulsed laser were carried out on<111>crystalline silicon wafers in this study. For each laser ablating process, final chemical composition and microstructural state of ablated material on sample surface were analyzed by X-ray photoelectron spectroscopy and transmission electron microscopy, respectively. Then the influences of laser pulse duration variation on the composition and microstructure of ablated material were also discussed. Therefore, the experimental results were considered to provide more completed and further understandings of laser-induced transitions of crystalline silicon, which may have some contribution to the development of laser-semiconductors micromachining.     

Nanopolishing of silicon wafers using ultrafine-dispersed diamonds

In the present study, two new methods are proposed for the polishing of silicon wafers using ultrafine-dispersed diamonds (UDDs). The first proposed polishing method uses a polishing tool with an ultrafine abrasive material made through the electrophoretic deposition of UDDs onto a brass rod. Dry polishing tests showed that the surface roughness of the silicon wafer was reduced from R_a=107 to 4 nm after polishing for 30 min. The second method uses a new polishing pad with self-generating porosity. By polishing with the new pad in combination with the polycrystalline UDD in a water suspension, it is possible to achieve the specified surface roughness of the silicon wafer much faster than when using a conventional pad made of foamed polyurethane. The tests showed that the surface roughness of the silicon wafer was reduced from R_a=107 to 2 nm after polishing for 90 min.     

Nanosecond laser-induced reshaping of periodic silicon nanostructures

We demonstrated the use of laser-induced reshaping to produce periodic silicon nanostructures (PSNs) with different geometries. Periodically located silicon nanostructures were preformed by dry etching of a silicon wafer covered with a monolayer of self-assembled polystyrene nanospheres. These PSNs were reshaped under ambient conditions by irradiation with two kinds of nanosecond lasers (532 nm and 355 nm). The effects of the irradiation parameters on the reshaped geometry were systematically investigated. Vertical growth of the irradiated PSNs resulted from the epitaxial deposition of rich silicon vapor during laser irradiation. However, the growth was limited even with higher laser fluence because of the nanoscale structure, the size of which is smaller than the melting depth induced by the nanosecond lasers. The reshaped PSNs displayed reflection spectra that are tunable by varying the characteristics of reshaping-laser input. This method offers a promising approach for the site-selective fabrication of optically tunable 3D nanostructures.     

Chemical characterisation by WD‐XRF and XRD of silicon carbide‐based grinding tools

This paper addresses the chemical characterisation of silicon carbide‐based grinding tools. These are among the most widely used grinding tools in the ceramic sector, and instruments are required that enable the grinding tool quality to be controlled, despite the considerable complexity involved in determining grinding tool chemical composition. They contain components of quite different nature, ranging from the silicon carbide abrasive to the resin binder. To develop the analysis method, grinding tools containing silicon carbide with different grain sizes were selected from different tile polishing stages. To develop the grinding tool characterisation method, the different measurement process steps were studied, from sample preparation, in which different milling methods (each appropriate for the relevant type of test) were used, to the optimisation of the determination of grinding tool components by spectroscopic and elemental analyses. For each technique, different particle sizes were used according to their needs. For elemental analysis, a sample below 150 µm was used, while for the rest of the determinations a sample below 60 µm was used. After milling, the crystalline phases were characterised by X‐ray powder diffraction and quantified using the Rietvel method. The different forms of carbon (organic carbon from the resin, inorganic carbon from the carbonates and carbon from the silicon carbide) were analysed using a series of elemental analyses. The other elements (Si, Al, Fe, Ca, Mg, Na, K, Ti, Mn, P and Cl) were determined by wavelength‐dispersive X‐ray fluorescence spectrometry, preparing the sample in the form of pressed pellets and fused beads. The chemical characterisation method developed was validated with mixtures of reference materials, as there are no reference materials of grinding tools available. This method can be used for quality control of silicon carbide‐based grinding tools. Copyright © 2010 John Wiley & Sons, Ltd.     

单晶硅表面均匀小尺寸金字塔制备及其特性研究

表面织构是一种通过有效的光俘获增加短路电流从而提高太阳电池效率的主要途径之一.在加入间隙式超声和NaClO添加剂的碱性四甲基氢氧化铵(TMAH)溶液中对单晶硅表面进行织构化处理,研究超声与NaClO在织构过程中对金字塔成核和生长的影响,以及金字塔大小对高温工艺之后的单晶硅少子寿命的影响.研究表明,通过在织构溶液中加入间隙式超声控制气泡停留在硅片表面的时间和脱离硅片表面速度,增强了小尺寸金字塔的均匀分布.织构之后硅片在AM1.5G光谱下的加权平均反射率能够达到12.4%,在高温扩散和氧化之后少子寿命的大小与金字塔大小之间存在近似于指数衰减函数的关系. 关键词： 表面织构化 反射率 少子寿命 单晶硅太阳电池     

Orientation of discotic and ferroelectric liquid crystals in a macroporous silicon matrix

Macroporous silicon with deep regular channels 3–4.5 μm in diameter was infiltrated with discotic and ferroelectric liquid crystals (LCs) at the temperature of the isotropic phase, and then, the system was slowly cooled to room temperature, with the liquid crystalline mesophase formed. The orientation of the LC molecules in the porous matrix was studied by FTIR spectroscopy. The alignment of LCs was ascertained by comparing the behavior of various vibrational bands of a liquid crystal introduced into the porous matrix with that for LC inside the bulk cells of planar and homeotropic alignment. The molecules of the discotic LC show a planar orientation of their column’s axis with respect to the surface of the macroporous silicon wafer; i.e., they are perpendicular to the channel axis. The long molecular axis of the ferroelectric LC is aligned with the pore walls, having homeotropic orientation with respect to the wafer surface. In a macroporous silicon matrix, both kinds of LCs show unexpected enhancement of the low-frequency vibrational bands. From Fizika Tverdogo Tela, Vol. 44, No. 6, 2002, pp. 1145–1150. Original English Text Copyright ? 2002 by Perova, Astrova, Tsvetkov, Tkachenko, Vij, Kumar. This article was submitted by the authors in English.     

Growth of iron single crystals in the etched ion tracks of polymer foils

Pulse reverse electrolysis in an ultrasonic field is used to grow iron single crystals of micron size in templates formed by etching the tracks of swift ions in polymer foils. High-grade crystals are produced from high-temperature ferrous chloride baths. The crystals are oriented along their <110>, <100>, and <111> crystallographic axes. Their orientation turns out to depend on supersaturation during the growing process. At low overvoltages of deposition, <110> and <100> orientations are observed. The crystals of <111> orientation appear more frequently at higher cathode pulse current density. The crystals possess prominent resistance to corrosion. Received: 20 February 2001 / Accepted: 21 February 2001 / Published online: 3 May 2001     

The effects of porous silicon on the crystalline properties of ZnO thin films

In the present work, ZnO was deposited on porous silicon substrates by sol-gel spin coating and rf magnetron sputtering. The porous silicon (PS) substrates were formed by electrochemical anodization on p-type (1 0 0) silicon wafer, and the starting material for ZnO was Zinc acetate dehydrate. Raman spectroscopy revealed the good quality of the porous silicon substrate. XRD analysis showed that highly (0 0 2) oriented ZnO thin films were formed. SEM, AFM and optical microscope have been used to understand the effects of the substrate on crystalline properties of the samples. The results indicated that the porous silicon substrate is beneficial to improve the crystalline quality in lattice mismatch heteroepitaxy due to its sponge-like structure.     

Numerical simulations of confocal Raman spectroscopic depth profiles of materials: a photon scattering approach

We present a simple model that uses a novel photon scattering approach to predict the depth profile response obtained when confocal Raman spectroscopy is applied both to silicon and to a number of related polymeric materials of varying optical clarity. This paper first provides an overview of the models proposed to date to demonstrate the evolution in understanding of the confocal Raman response of semi‐transparent materials, based upon geometrical optics. A new model is then described that is based upon the twin notions of a permanent extended Raman illuminated volume and the degree of extinction of the incident and Raman scattered photons from the whole of the illuminated volume as it is gradually moved further into, or defocused above, the sample. The model's predictions are compared with empirical data from previous studies of a range of semi‐crystalline polymers with different scattering properties and, by means of contrast, with that of a silicon sample. We show that, despite its inherent simplicity, the physics this model utilizes is able successfully to predict the form of the depth profile for each material, something that has not been achieved by any model previously proposed, and that the parameters used in the model scale with independent physical measurements. Finally the model is used to account for the fact that useful Raman spectra can be obtained when the laser is focused as much as 40 µm above the sample surface. Copyright © 2007 John Wiley & Sons, Ltd.     

Slip damage of silicon wafers subjected to continuous infrared laser irradiation

Laser irradiation can cause damage to solids, such as slipping, cracking, melting, and ablation. Silicon crystals are brittle, so slipping is a serious problem because it can easily result in fracture. This study investigates the amount of continuous near-infrared (NIR) laser irradiance that induces slip damage in a single-crystal silicon wafer. For this purpose we developed a simulation model based on heat transfer and thermo-elastic analyses. To verify the simulation model, silicon wafer specimens were irradiated by a fiber laser beam (of wavelength 1065 nm), and the surface morphology after laser beam irradiation was inspected using optical microscopy (OM). The irradiation time was fixed at 10 s, and nine different irradiances from 180 W/cm² to 380 W/cm² were tested in steps of 25 W/cm². No slip surface was found after exposure to the irradiances up to 230 W/cm², but straight slips in the <110> direction appeared at the irradiances of 255 W/cm² and above. These experimental findings agreed well with the simulation.