High sensitive electrolytical conductivity measurements of irradiated polymer films of 1μm thickness measured by a modified experimental set-up

The interaction of heavy ions with solids produces a narrow radial core of primary damage. The actual nature of the damage and the mechanism of its formation is not yet fully understood.

The technique of the electrochemical etching of irradiated samples is an useful method to investigate these structures of the track cores. The transversale etching rate as a function of the radius, derived from the time-dependence of the radius of the etching pore, can be interpreted as the corresponding magnitude of the degree of the damage within the track core.

To carry through measurements of smallest radii of etching pores, their very high electric resistance respectively, a sophisticated experimental set-up is required.

An advanced set-up is performed, which enables, by application of a combined d.c.-a.c.-method, to measure the resistance of the sample during the whole etching process, associated with the origin of pore and its growth up to radii of 10 nm and more.     

Empirical relationship between track diameter and etching time for fission fragments incident on a glass SSNTD at various angles of incidence

Geometrical shapes and diameter of nuclear tracks changes continuously during the process of etching for various incident angles. Besides, there is also a marked difference amongst their profiles, as evidenced by the SEM analysis, when the incoming particles fall on the detector at different angles of incidence. This work outlines this aspect of fission fragment tracks in a glass detector and has set out a few empirical relationship between the mean track diameter, d, and the etching time, t, within experimental limits. This study, therefore, sheds some light in the follow up the origins and chracteristics of heavy ions in some terrestrial and extra-terrestrial materials and also in studying the collimation accuracy of heavy ion bombardments. The implications of the results in discerning the measurements of incident angles of various types of ions are described in detail in the paper.     

基于智能算法的CR39径迹刻蚀过程模拟

CR39可以用于激光等离子物理实验中的离子探测,并给出离子数目、种类和能量信息。通过采用唯象模型,利用离子在CR39中径迹形成的阻止本领动力学方程以及粒子群智能算法对径迹形成的过程进行了数值化模拟,研究了CR39中离子径迹在刻蚀过程中的演化过程,获得了入射离子能量和径迹直径、深度的对应关系,并且发现当离子射程与刻蚀深度相等时,径迹深度最大,给出了利用总刻蚀时间计算最大径迹深度对应的临界能量的公式。     

Electrolytes in etching of latent tracks of heavy ions in polyethylene terephthalate

Previously unknown features of etching of polyethylene terephthalate, latent tracks of multiply charged accelerated ions in it, and track membrane pore formation are considered. It was found that K ions (in the form of KCl salt) in a KOH solution enhance etching of both initial polyethylene terephthalate and tracks. Ba²⁺ ions enhancing etching of initial polymer significantly inhibit etching of tracks. It is assumed that etching inhibition is associated with Ba²⁺ ion adsorption on track active centers. The features detected are used to fabricate track membranes with thin selective layer.     

~(32)S离子辐照PET薄膜制备亚微米孔径核孔膜研究

使用中国原子能科学研究院HI-13串列加速器产生的32S离子轰击BOPET薄膜,薄膜在空气中陈化3个月后在专用装置中使用Na OH溶液蚀刻制备核孔膜,研究Na OH溶液浓度、蚀刻温度对微孔孔形的影响。在不同温度和蚀刻液浓度条件下,蚀刻出微孔孔径为0.2至0.93μm的亚微米核孔膜,计算其微孔锥角,得出微孔锥角随着蚀刻温度、蚀刻液浓度和微孔孔径的变化趋势。研究表明,采用低浓度、高温度的Na OH溶液蚀刻有利于减小微孔锥角,有利于制备较小孔径的核孔膜。如选用0.5mol/L的Na OH溶液浓度,在蚀刻温度为90℃的条件下蚀刻,此时蚀刻时间小于2 h,既可以得到高质量微孔膜也有利于提高生产效率。     

Energy transport in plasma etching of nanoporous dielectric materials

A Monte Carlo routine was developed to simulate the motion and energetics of ions in the pores of a xerogel material under plasma etching conditions. The simulation included the effects of an applied electric field and input conditions for the pore as a function of pressure and applied voltage in the plasma reactor. We were interested in the ion energy in a pore, the ion penetration depth and the effect of ion energy on etching.At low pressures the nanoporous material etches faster than dense silicon dioxide. This is to be expected given the decrease in density and increase in surface area that arises due to the porosity. However, as the pressure is increased, the etch rate decreases dramatically and, eventually, the dense oxide may etch faster than the porous material. CHF₃ was used as the etchant gas and, for this gas, we believe this behavior to be controlled by the ion energy and energy transport in the pores of the xerogel material. As the pressure in the plasma reactor is increased, the incoming ions switch over from etching activation to polymerisation activation. This agrees with the observed crossover in etch rate seen experimentally and with the cessation in etching as pressure is increased. The switch is affected by pore roughness and correlates with the average ion energy in the pore.     

Self assembled micro masking effect in the fabrication of SiC nanopillars by ICP-RIE dry etching

This report presents the results of the novel fabrication of 4H-SiC pillars with nanopores using ICP-RIE dry etching. Cl₂/Ar gas plasma with various mass flow rates was used in this etching process to produce SiC nanopillars without using patterned etch mask. Cylindrical pillars of 300 nm diameter and 500 nm height with smooth side walls were etched on SiC wafer. The etching condition for the optimized fabrication of SiC nanopillars is presented in this report. Each nanopillar has been produced with a nanosize pore at the center along its length and up to the middle of the cylindrical nanopillar; it is a unique feature has not ever been reported in case of SiC. Inclusion of oxygen was found influence the formation of nanopillars by the effect of SiO₂ micro masking. The formation of self assembled SiO₂ layer and its micro masking effect in the fabrication of this unique nanostructure has been investigated using TEM, STEM and EDAX measurements.     

Design of a multifoil electrolytically controlled etching cell

Irradiating polymer films with heavy ions and subsequent electrolytically controlled etching (ECE) produces nuclear track filters with desired pore dimensions and pore density. During ECE, an electric field with low field strength and a frequency in the audio range is applied across the irradiated polymer film, which is immersed in the etching solution. An ECE cell for the simultaneous etching of three irradiated samples has been designed and developed. The average pore diameter and break-through time for tracks due to ²³⁸U(11.4 and 14 MeV/u) and ²⁰⁹Bi(13 MeV/u) ions in polycarbonate and polyethylene terepthalate have been measured.     

High Energy Charged Particle Registration in CR-39 Polycarbonated Detector

Track etch rate characteristics of CR-39 plastic detector exposed to ²⁸Si ions of 670 MeV energy have been investigated. Experimental results were obtained in terms of frequency distribution of the track diameter, track density and bulk etching rate. A dependence of the mean track diameter on energy was found. The application of the radiation effect of heavy ions on CR-39 in the field of radiation detection and dosimetry are discussed. Results indicated that it is possible to produce etchable tracks of ²⁸Si in this energy range in CR-39. We also report the etching characteristics of these tracks in the CR-39 detector.     

The statistical process of pore growth in multi pore foils

Using the electrolytical etching method the breakthrough-times (i.e. the time when the two etched cones from both sides of the detector contact) and the resulting track etching rates v_t of heavy ion tracks in 8 μm polycarbonate Makrofol KG have been measured. The samples were irradiated at the GSI, Darmstadt (Germany) with gold ions and different fluences at a specific energy of 11.6 MeV/u. All foils were etched in 6 n NaOH at room temperature. Fluctuations of breakthrough-times of single pore foils were analysed. Also the breakthrough-time of multi-pore-foils were measured. The dependence of the mean breakthrough-time on the ion fluence is dicussed. This dependence will be explained by the fluctuations of the breakthrough-time of the pores.     

Applications of porous silicon formed by electrochemical etching using an electrolyte based on HF:formaldehyde

In this work, we report the experimental results on the formation of porous silicon (PSi) monolayers by electrochemical etching using a formaldehyde based electrolyte. The results were compared with PSi monolayers obtained with the traditional electrolyte (HF:ethanol). Both electrolytes facilitate the removal of H₂ generated as a subproduct during the electrochemical etching process in the surface of the c-Si substrate. Formaldehyde presents a good affinity to surfaces and interfaces and the excess of water in the electrolyte reduces the pore sizes of PSi samples. The porosity and etching rate values are similar than those obtained using HF:et solutions. The refractive index values are the same in both cases at the same porosity in the visible range. The results have shown that the chemical characteristics of the ethanol and formaldehyde can give some different advantages to the PSi process and its applications.     

The pore opening process of etching polymer films irradiated by single and multiple heavy ions. The etching process in the range of the track core radius (10 nm)

The technique of electrochemical etching of irradiated polymer films is an useful method to investigate structures of the track cores. In the case of the investigation of multiple track foils, the mean effective radius corresponds to the average of all synchron etching pores. On the other hand, the etching cones of all tracks do not break through to conducting micro channels coincidentally. The statistical character of this pore opening (break through) process is still unexplained, although several effects concerning this topic have been observed in the past. Another computer program simulates by way of the Monte Carlo Method the etching process of an ensemble of tracks within a thin polymer film. The conductivity of the multiple track etching foil can be described by the convolution between the conductivity of a single pore and the time dependent breakthrough rate. By way of the Laplace Transforms the measurements of the multiple and single track etching polymer films can be deconvoluted and yield the statistical nature of the pore opening process.     

Nanoporous silicon fabricated at different illumination and electrochemical conditions

The properties of porous silicon prepared at different illumination and electrochemical conditions were studied. The preparation procedure was based on the electrochemical etching in HF containing electrolyte. In the dissolution of n-type silicon, an external source of light is necessary to obtain a sufficient holes flux density. Here, illumination was applied from the backside of the wafer (the side not immersed in the electrolyte), from topside (the side immersed in the electrolyte), and for the highly doped silicon, etching proceeds without illumination. The electrolyte contains HF in the range 2–50 wt%. The highest current density flows with topside assisted illumination. Backside illumination and etching in the dark resulted in a reduction in the current density. In the dark the current density significantly increased at a higher anodic bias. These conditions gave rise to pores formation with a diameter from 20 nm up to 3 μm. The smallest pore size was obtained for highly doped n-Si (111) wafers, etched without illumination. The present paper confirms the possibility of porous silicon formation in the dark and with backside illumination, these being alternative methods for topside assisted illumination etching methods.     

The pore opening process and its influence on conductivity measurements of irradiated polymer films by application of the electrochemical etching method

The technique of the electrochemical etching of irradiated polymer films is an useful method to investigate structures of the track cores.

The transversale etching rate as a function of the radius, derived from the time-dependence of the radius of the etching pore, can be interpreted as a corresponding magnitude of the degree of the damage within the track core.

In the case of polymer films irradiated by a high track density, the influence of the time distribution of the breakthroughs (pore opening process) of the etching microchannels on the conductivity changes during the etching process is to be discussed. First represented results lead to statements about the statistical nature of the pore opening process.     

电化学方法制备Si阵列微孔的工艺研究

对用电化学方法制备Si大孔阵列管坑工艺进行了初步探索。 通过对Si在KOH溶液中各向异性湿法蚀刻和在HF酸溶液中的电化学蚀刻过程中各种参数的摸索, 确定在室温下制备大孔阵列的最佳配比浓度, 蚀刻出符合要求的管坑阵列, 为进一步制备结构化闪烁屏奠定了实验基础。 The 3 D structures in silicon are increasingly coming to use in many fields. For example, the high resolution X ray digital imaging detector can be made by coupling CCD and the scintillating screen which is made by the array trenches filled with CsI(Tl). In the present work, we explored the technology of etching micro array on the n type silicon with high resistance. By studying the relative parameters of anisotropic etching of KOH and electro chemical etching of HF, the optimized concentration of HF was determined and the micro pore array trenches with 200 μm in depth were realized. The results establish an experimental base for further fabrication of the scintillating screen.     

The influence of the gas cluster ion beam composition on defect formation in targets

Defect formation in silicon-on-sapphire films under the action of a gas beam of 30 keV argon cluster ions is studied. Rutherford backscattering in the channeling mode is used to demonstrate the formation of a large number of defects in the volume of a specimen that is irradiated by a cluster ion beam without mass separation. If atomic and light cluster ions are removed from the beam, defect-free etching of the specimen occurs.     

Monte Carlo simulation of radon SSNT detectors

A Monte Carlo based software for the computation of the sensitivity of etched radon track detectors was developed. It can be applied to the measurement of radon and radon daughters in free air or inside of a measurement chamber. LR 115 and CR-39 detectors, with or without an attenuator, are specifically addressed. Various etching conditions and observation criteria for counting the track density may be specified. The latent track formation and the etching process are realistically modelled. The dependence of the etch-rate ratio on the energy is taken into account. The plate-out phenomenon is included in the model. An inhomogeneous source distribution in the detector cup can be considered.     

Study of inhomogeneity in thickness of LR 115 detector with SEM and Form Talysurf

Long-term measurements of radon progeny concentrations using Solid-State nuclear tract detector are being actively explored. These measurements depend critically on the thickness of the removed layer during etching. Scanning electron microscope (SEM) observations have identified irregularities in etched LR 115 detectors, such as detachment of the active layer from the substrate and formation of air gaps in the substrate. After discarding these irregularities, by using “Form Talysurf” surface profile measurements, the thickness of the active layers for the LR 115 detector are found to be 11.8±0.2 and 5.0±0.4 μm before and after 2 h of etching, respectively. The coefficient of variation has thus risen from 1.7% to 8.0% on etching. The increased inhomogeneity is explained by the formation of track-like damages, which have been observed using Form Talysurf, SEM, optical microscope and atomic force microscope. With this relative large coefficient of variation, the thickness of the active layer in the LR 115 detector cannot be assumed to be homogeneous in general, and the associated uncertainties should be considered carefully when the detector is used for alpha spectroscopy.     

The study of the solution concentration influencing on laser-induced electrochemical etching silicon

The laser electrochemical etching process, which combines the laser direct etching process and the electrochemical etching process, is a compound etching technique. In order to further understand the solution concentration influencing on the laser-induced electrochemical etching of silicon; a 248 nm excimer laser as a light source and KOH solution as an electrolyte were adopted in this study. The experiments of micromachining silicon by laser-induced electrochemical etching were carried out. On the basis of the experiments results, the solution concentration influencing on the etching rates in the process of laser electrochemical etching of silicon was researched. The reasons of the etching phenomena were analyzed in detail. The experimental results indicate that the solution concentration influencing on the etching process is mainly rooted in the absorption of different concentration solutions to laser. In general, less absorption and low solution concentration are good for the etching role in the process of laser electrochemical etching.