Ion track etching revisited: II. Electronic properties of aged tracks in polymers

We compile here electronic ion track etching effects, such as capacitive-type currents, current spike emission, phase shift, rectification and background currents that eventually emerge upon application of sinusoidal alternating voltages across thin, aged swift heavy ion-irradiated polymer foils during etching. Both capacitive-type currents and current spike emission occur as long as obstacles still prevent a smooth continuous charge carrier passage across the foils. In the case of sufficiently high applied electric fields, these obstacles are overcome by spike emission. These effects vanish upon etchant breakthrough. Subsequent transmitted currents are usually of Ohmic type, but shortly after breakthrough (during the track’ core etching) often still exhibit deviations such as strong positive phase shifts. They stem from very slow charge carrier mobility across the etched ion tracks due to retarding trapping/detrapping processes. Upon etching the track’s penumbra, one occasionally observes a split-up into two transmitted current components, one with positive and another one with negative phase shifts. Usually, these phase shifts vanish when bulk etching starts. Current rectification upon track etching is a very frequent phenomenon. Rectification uses to inverse when core etching ends and penumbra etching begins. When the latter ends, rectification largely vanishes. Occasionally, some residual rectification remains which we attribute to the aged polymeric bulk itself. Last not least, we still consider background currents which often emerge transiently during track etching. We could assign them clearly to differences in the electrochemical potential of the liquids on both sides of the etched polymer foils. Transient relaxation effects during the track etching cause their eventually chaotic behaviour.     

Use of chemical etching of CR-39 foils at elevated temperature for fast neutron personnel monitoring in India

CR-39 Solid State Nuclear Track Detecting foils (SSNTD), along with 1 mm thick polyethylene radiator, sealed in triple laminated pouches, are used for country wide Fast Neutron Personnel Monitoring in India. With the present system of processing by elevated temperature electrochemical etching (ETECE) and evaluation using automatic image analysis, only 16 foils are processed at a time and it is useful over the dose equivalent range 0.2 mSv to 10 mSv. It has been reported that, by processing CR-39 of good detection efficiency by chemical etching at elevated temperature, more numbers of foils can be processed simultaneously. In the present study, CR-39 foils from Pershore Moulding (UK) have been chemically etched using 7 N KOH under various conditions of temperature and etching durations and evaluated using high magnification microscope. The duration of chemical etching, has been optimized at a constant temperature of 60°C for chemical etching process. The characteristics of the chemically etched CR-39 foils are compared with the characteristics of the CR-39 foils processed by the existing system of ETECE and the detailed results are presented in the full text of the paper. It has been observed that by chemical etching process, the dose equivalent range of CR-39 foils can be extended above 60 mSv.      

Energy loss dependent transversal etching rates of heavy ion tracks in plastic

By the method of electrolytical etching track etching rates V_t and corresponding transversal track etching rates V_trans of single heavy ion tracks in thin Makrofol KG foils have been measured at ion energies from 10–480 MeV/u. Makrofol KG foils of 8 μm thickness were irradiated perpendicular to the surface with ⁷⁹Au and ⁵⁴Xe ions at specific energies with energy loss values of REL=(10–90) ^*10³ MeVcm²/g at GSI Darmstadt, Germany, and Lawrence Berkeley Lab., Cal., USA. Using the electrolytical etching method by measuring the resistance of the foil during the etching process (etching conditions: 6n NaOH, room temperature and controlled 50° C) the breakthrough time and track etching rates V_t, V_trans and V_m (bulk etching rate) were analysed. Response curves (V_t/V_m)-1 as a function of Restricted Energy Loss (REL), the maximum extension of the ion induced damage perpendicular to the ion path and the dimension of the ion track core depending on the deposited energy can be estimated.     

Study of current drain during electrochemical etching of polycarbonate detectors

Polycarbonate (PC) detector is one of the common detectors for neutron and radon gas detection. Using this detector it is possible to measure the dose in mSv, by counting tracks/cm² on an etched surface. In this paper, a special procedure has been suggested to determine the dose based on current drain during the etching process. In these experiments the effects of voltage, frequency, effective etched area, PC detector's thickness, etched area (one side or two sides), etching solution temperature and dose absorbed by the PC foil have been studied.The results obtained show the current drain variation for a voltage of 200–1600 V, a frequency of 2–10 kHz, effective area with a diameter of 2–12 cm, PC thickness of 125–250–375– and a temperature of etching solution of 25–.Lexan PC foils were exposed to doses of of neutrons. The unexposed foils were considered as the background (BG) foils. Most of the experiments were performed at a voltage of 800 V, a frequency of 2 and 8 kHz, foil thickness of , diameter of effective etched area of foils of 2, 6 and 12 cm, temperatures of 25 and and the etching process from 0 up to overload stage. Overload stage occurs when the foil becomes so thin due to growth of the tracks that it leads to sparking between phase and null that makes a hole in the foil.Current drain curves versus the function of the etching time are absolutely different for various doses from zero (BG) to 10 rad (BG up to ). This is true especially for the time interval from 3 h of etching up to overload stage. In this way, it is possible to obtain a calibration of PC detector net current drain based on its absorbed dose.In this experiment, the number and diameter of tracks and their relation with drain current and PC foil residual thickness at overload stage have been studied.The same experiment has been performed for various concentrations of radon gas (Bq/m3) as well.     

Coupled chemical reactions in dynamic nanometric confinement: Ag2O membrane formation during ion track etching

In this study, continuous swift heavy ion tracks in thin polymer foils were etched from both sides to create two conical nanopores opposing each other. Shortly before both cones merged, one of the nanopores was filled with a silver salt solution, whereas etching of the other cone continued. At the moment of track breakthrough, the etchant reacted with the silver salt solution by forming an impermeable and insulating membrane. Continued etching around the thus-created obstacle led to repetitive {etchant – silver salt solution} interactions. The coupling of the two chemical reactions, {etchant – polymer} and {etchant – silver salt solution}, within the confinement of etched tracks, with continuously changing shapes, showed a highly dynamic nature as recorded by measuring both the electrical current and the optical transmission across the foils. At low etching speeds, a central membrane that grew in radius and thickness with time until, at a critical thickness, the membrane became rather impermeable was formed. However, at high etching speeds, the emerging reaction products exhibited a sponge-like consistency, which allowed for their infinite growth. This precipitation was accompanied by a pronounced current spike formation. A simple theoretical model explains, at a minimum, the basic features.     

Comparison of responses of CR-39, PM-355, and CN track detectors to energetic hydrogen-, helium-, nitrogen-, and oxygen-ions

Samples made of the CR-39 and PM-355 plastic nuclear track detectors (NTDs) as well as of the CN films were irradiated with quasi-monoenergetic beams of protons, alphas, N⁺-, and O⁺-ions produced by various accelerators. For different samples an energy value of the particle beams was changed from several hundreds keV to 3 or 4.5 MeV. After irradiation the detector samples were etched chemically under controlled conditions during periods lasting from 2 hrs to 20 hrs. Every 2 hrs track diameters were measured by means of an optical microscope. Differences in the crater diameters in the detectors etched in steps, and those etched continously, have been found to be smaller than 10 percent. The paper results detailed calibration diagrams showing a dependence of track diameters on the ion energy value for different etching times.     

Laser backside etching of fused silica with ultra-short pulses

Laser backside etching of transparent materials like fused silica at the interface to liquids with sub-picosecond UV laser pulses using a pyrene/toluene solution is achieved. For the experimental conditions applied, the etching effect is rather weak with measured rates of the order of 0.1 nm/pulse. A linear dependence of the etched volume upon the laser pulse energy or the pulse number was extracted from the experimental data obtained. At low pulse numbers the etched surface exhibits a feature-free, smooth morphology, while quasi-periodic ripple formation is observed for prolonged laser exposure. In addition, the etching process is accompanied by enhanced carbon deposition at and in the vicinity of the etched surface. The etching mechanism proposed comprises the primary interaction of the laser radiation with the liquid, a surface-modification phase, and the etching of the modified fused-silica surface. PACS 81.65.Cf; 81.05.Kf; 79.20.Ds; 61.80.Ba; 42.55.Lt; 68.45.Da     

Electro-responsive asymmetric nanopores in polyimide with stable ion-current signal

For the preparation of a single asymmetrically shaped nanopore in a polyimide membrane, Kapton foils were irradiated with single heavy ions and subsequently etched from one side in sodium hypochlorite (NaOCl). The other side of the membrane was protected from etching by a stopping medium containing a reducing agent for hypochlorite ions (OCl^-). The resulting conical nanopore rectified ion current and exhibited a stable ion-current flow. Received: 23 May 2002 / Accepted: 2 September 2002 / Published online: 15 January 2003 RID="*" ID="*"Corresponding author. Fax: +49-6159/712-179, E-mail: Z.Siwy@gsi.de     

SHI induced nano track polymer filters and characterization

Swift heavy ion irradiation produces damage in polymers in the form of latent tracks. Latent tracks can be enlarged by etching it in a suitable etchant and thus nuclear track etch membrane can be formed for gas permeation / purification in particular for hydrogen where the molecular size is very small. By applying suitable and controlled etching conditions well defined tracks can be formed for specific applications of the membranes. After etching gas permeation method is used for characterizing the tracks. In the present work polycarbonate (PC) of various thickness were irradiated with energetic ion beam at Inter University Accelerator Centre (IUAC), New Delhi. Nuclear tracks were modified by etching the PC in 6N NaOH at 60 (±1) °C from both sides for different times to produce track etch membranes. At critical etch time the etched pits from both the sides meet a rapid increase in gas permeation was observed. Permeability of hydrogen and carbon dioxide has been measured in samples etched for different times. The latent tracks produced by SHI irradiation in the track etch membranes show enhancement of free volume of the polymer. Nano filters are separation devices for the mixture of gases, different ions in the solution and isotopes and isobars separations. The polymer thin films with controlled porosity finding it self as best choice. However, the permeability and selectivity of these polymer based membrane filters are very important at the nano scale separation. The Swift Heavy Ion (SHI) induced nuclear track etched polymeric films with controlled etching have been attempted and characterized as nano scale filters.      

A study of the basic properties of electrochemical track etching

The basic properties of the electrochemical track etching method proposed by Tommasino were studied for PC and PET foils irradiated with fission fragments and/or alpha-particles. Etching was performed in a specially designed double-wall vessel applying electric fields of different strengths and frequencies. The variation in the diameters of the discharge spots produced around the tracks of fission fragments entering PC and PET foils at right angles was systematically studied as a function of the strength and frequency of the electric field, etching time and etchant temperature. For alpha-tracks registered in PC foils the dependence of the discharge spot diameter on particle energy was also determined. It was found that the production of discharge spots started at a threshold field strength depending on the type of particle. The temperature dependence of the growing rate of discharge spots followed the Arrhenius law, but with a reduced activation energy as compared to that obtained for the chemical etching rate of the bulk material.     

Coupled chemical reactions in dynamic nanometric confinement: V. The influence of Li+ and F− ions on etching of nuclear tracks in polymers

Etching of continuous nuclear tracks in thin polymer foils from both sides is known to lead to the formation of double-conical nanopores. In this work and related ones we try to find out how this etching kinetics is modified when materials are added which react with each other upon their contact towards some new product that influences the etching. For that purpose we have chosen here Li⁺ and F^? ions as the additions, which react with each other to form LiF precipitations. The coupled etching and precipitation kinetics is recorded by measuring the electrical current that is transmitted through the foils upon application of a low-frequency alternating sinusoidal voltage. Depending on the etchant concentrations, the etching temperature and the time of Li⁺ and F^? addition, different effects are found that range from (a) no alteration of the transmitted current at all, via (b) the emergence of an alternating current with a temperature-dependent amplitude, and (c) the complete vanishing of any transmitted current at all, towards (d) chaotic transmitted current histories with phases with strong current spike emission and (e) rather quiet phases, alternating with each other in a rather unsystematic way. The observed effects are ascribed to (a) the enhanced penetration efficiency of both the Li⁺ and F^? ions through the polymeric bulk and/or latent ion tracks after the removal of the polymer's protective surface layer by the etchant, (b) the high mobility of preferentially the F^? ions within the polymer, (c) the LiF precipitation within the polymer or on its surface upon encounter of Li⁺ and F^? ions, (d) the nanofluidic properties of narrow etched tracks covered with Li⁺ ions on the wall surfaces and F^? ions beyond, and/or (e) the formation of LiF membranes within the etched tracks.     

惯性约束聚变实验用平面薄膜的制备及其表面图形的引入

平面薄膜是ICF分解实验的重要靶型,以半导体技术结合重掺杂自截止腐蚀制备厚度为3－4um的Si平面薄膜,以热蒸发结合脱膜工艺制备Al平面薄膜,两者的表面粗糙度分别为30nm和10nm左右;进一步采用离子束刻蚀在平面薄膜的表面引入网格或条状图形,获得测量成像系统像传递函数的刻蚀膜,控制离子束刻蚀工艺的参数以实现图形的精确转移。     

Effect of temperature and silicon resistivity on the elaboration of silicon nanowires by electroless etching

The morphology of silicon nanowire (SiNW) layers formed by Ag-assisted electroless etching in HF/H₂O₂ solution was studied. Prior to the etching, the Ag nanoparticles were deposited on p-type Si(1 0 0) wafers by electroless metal deposition (EMD) in HF/AgNO₃ solution at room temperature. The effect of etching temperature and silicon resistivity on the formation process of nanowires was studied. The secondary ion mass spectra (SIMS) technique is used to study the penetration of silver in the etched layers. The morphology of etched layers was investigated by scanning electron microscope (SEM).     

Thermochemical dry etching of single crystal ferrite by laser irradiation in CCl4 gas atmosphere

Single crystal ferrite has been etched by focused Ar⁺ laser irradiation in a CCl₄ gas atmosphere. The etched groove showed cracks due to thermal stresses when samples were etched by a laser vaporization process in a vacuum, while in a CCl₄ atmosphere, such cracks were not observed. An etching rate of 68 /s obtained for a thermochemical process by laser irradiation was four orders of magnitude higher than that for a wet chemical etching process. A high aspect (depth-to-width) ratio of up to 10 was obtained for etched grooves. Under specific conditions, bending of the groove and orientation dependence in etching rate were observed.     

离子径迹模板法制备纳米线

重离子辐照的高分子有机膜,经过适当的处理,可以作为模板制备金属和可溶性盐纳米线,此方法称为离子径迹模板法。介绍了用电化学沉积方法和过饱和溶液法制备金属纳米线和可溶性盐纳米线的基本原理和制各实例,同时还展望了离子径迹模板法制备纳米线的一些可能的应用。The polymer foils irradiated by heavy ions can be used as temptates to prepai nanowires and some inorganic salt nanowires. It is called ＂ion-track template method＂. Compared to other templates, such as AAO template and porous silicon, etched ion-track template is more convenient and flexible. The density of the pores can be easily controlled by changing the ion fluences and the diameter of the pores can be altered through changing the etching condition. The pores of the etched ion-track template are well aligned. We present some examples of preparing metallic nanowires and inorganic salt wires by electrochemical deposition and by supersaturation solution method, respectively. We also introduce some applications of nanowires prepared with ion-track template method.     

Highly regular nanometer-sized hexagonal pipes in 6H-SiC(0001)

An array of troughs was prepared on a 6H-SiC(0001) surface using focused ion beam (FIB) patterning. Troughs were etched with various ion doses and close-to-circular voids of increasing depths for larger ion doses were obtained. The samples were then etched in a hot-wall reactor at a hydrogen partial pressure of 13 mbar at 1800 °C. The resulting morphological reorganizations have been studied by scanning electron and atomic force microscopy. Very regular hexagonal voids with facets oriented perpendicular to the surface were obtained after hydrogen etching. The voids were surrounded by regular secondary facets of lower inclination. Whereas the depth of the voids increases with ion dose, the void diameter and facet sizes stay constant. This effect is explained by surface diffusion during hydrogen etching. The FIB technique in combination with hydrogen etching allows the preparation of very regular surface patterns and highly ordered wells and tubes for nanometer-sized sieves and photonic crystals. PACS 47.70.Fw; 68.37.-d; 68.37.Hk; 68.37.Ps; 81.65.Cf     

Investigation of response of CR-39, PM-355 and PM-500 types of nuclear track detectors to energetic carbon ions

Samples of CR-39, PM-355, and PM-500 plastic detectors were irradiated with carbon ions of energy ranging from 0.9 MeV to 14.7 MeV. After the irradiation the detector samples were etched for a period from 2 hrs to 10 hrs. Dependence of track diameters on the ion energy values for different etching times, and dependence of V_T/V_B as a function of incident carbon-ion energy, are presented.     

Observation of diffusion through ion irradiated Makrofol KG

The features of the latent track in polycarbonate can be analysed by measuring the diffusion constant under ultra high vacuum conditions. Stacks of 30 μm Makrofol KG foils were irradiated with uranium ions of 11.4 MeV/u at the GSI Darmstadt, Germany. We used different fluences from 3·10¹⁰ to 5·10¹¹ ions/cm². The diffusion constant was determined by the time-lag-method [1]. A quadrupole mass filter was used to observe the diffusion of the gas. We measured the diffusion of argon through different foils of each stack at room temperature. In all cases also unirradiated foils were measured. The dependence of the permeability and the diffusion constant on the ion fluence and the energy loss of the ions will be given and indications on the size of latent ion tracks concerning gas diffusion will be discussed.     

Modification of plasma-etched profiles by sputtering

Two-dimensional etch profiles are modeled for plasma etching. The etch rate dependence on the angle of incidence of the bombarding ions on the etched surface has a sputtering-type yield. The etch profile is advanced in time by an evolution equation for an etch rate proportional to the modified ion energy flux. Approximate analytical expressions for the etch rates are derived as a product of the etch rates in the absence of the sputtering-type yield and a weighting factor that depends on the angle the ion drift velocity makes with the normal to the wafer surface. The weighting factor is determined from experimental measurements of the angular dependence of ion beam etching by sputtering. These etch rates are valid when the ratio of the ion drift speed to the ion thermal speed is large compared to one. The etching is modeled in the ion flux-limited regime for simplicity. The modifications of the shape of etch profiles of a long rectangular trench and a waveguide structure or strip are treated     

In situ reflectivity investigations of solid/liquid interface during laser backside etching

In situ reflectivity measurements of the solid/liquid interface with a pump-probe setup were performed during laser-induced backside wet etching (LIBWE) of fused silica with KrF excimer laser using toluene as absorbing liquid. The intensity, the temporal shape, and the duration of the reflected light measured in dependence on the laser fluence are discussed referring to the surface modification and the bubble formation.The vaporisation of the superheated liquid at the solid interface causes a considerable increase of the reflectivity and gives information about the bubble lifetime. The alterations of the reflectivity after bubbles collapse can be explained with the changed optical properties due to surface modifications of the solid surface. Comparative studies of the reflectivity at different times and the etch rate behaviour in dependence on the laser fluence show that the in situ measured surface modification begins just at the etch threshold fluence and correlates further with etch rate behaviour and the etched surface appearance. The already observed surface modification at LIBWE due to a carbon deposition and structural changes of the near surface region are approved by the changes of the interface reflectivity and emphasizes the importance of the modified surface region in the laser-induced backside wet etching process.