Detection of fission tracks on resin plates formed from three kinds of DAP monomers

This work compares the response properties of ortho, meta and para diallyl phthalate (DAP) resin plates and their copolymer plates cast under the same curing conditions. The plates were irradiated with fission fragments and alpha-particles. After irradiation, the plates were etched with a potassium hydroxide, ethanol and water (PEW) solution or an aqueous solution of potassium hydroxide. Enlarged nuclear tracks were observed and counted using an optical microscope. All plates were found to have a detection efficiency of almost 100% for fission fragments, and yet were found to be insensitive to alpha-particles. From the experimental results of finish in curing, ease in cutting, etching speed and heat resistance, the ortho-based plates have been found to be superior to the meta- or para-based plates as a fission track detector.     

Characteristics of diallyl phthalate resin as a fission track detector

Diallyl phthalate (DAP) resin plates were irradiated with fission fragments, and then etched in aqueous solution of KOH. Etched tracks were observed and counted by using an optical microscope. The detection efficiency of fission fragments was about 100% for both perpendicular and random incidence. DAP plates were insensitive to alpha particles and fast neutrons. These characteristics are suitable for detecting selected fission fragments, which coexist with alpha particles or fast neutrons. DAP plates are valuable for quantitative analysis of fissionable materials and neutron dosimetry. DAP and allyl diglycol carbonate (CR-39) were formed into copolymers in various ratios. The copolymers showed intermediate characteristics between DAP and CR-39. The fabrication of the copolymers made it possible to control the discrimination level for detection of heavy charged particles.     

Diallyl phthalate resin and its copolymers containing allyl diglycol carbonate as nuclear track detectors

Diallyl phthalate (DAP) and allyl diglycol carbonate (CR-39), and mixtures of DAP and CR-39 were cast into plates under the same polymerizing conditions. The plates were irradiated with alpha-particles, fission fragments or fast neutrons. After etching, enlarged tracks on the plates were observed and counted using an optical microscope. Pure DAP plate was found to have high detection efficiency for fission fragments, but to be insensitive to alpha-particles and fast neutrons. This characteristic was suitable for detecting fission fragments. On the other hand, pure CR-39 plate was convenient for the detection of alpha-particles and fast neutrons because of high detection efficiency and sensitivity, and short etching time. The copolymers of DAP and CR-39 showed intermediate characteristics. The fabrication of the copolymers made it possible to control the discrimination level for the detection of heavy charged particles.     

Micro‐Raman spectroscopy and SEM/EDX applied to improve the zircon fission track method used for dating geological formations

The zircon mineral is widely studied in geochronology. In the case of the fission track method (FTM), the age is determined by the density of fission tracks at the zircon surface, which can be observed with an optical microscope after an appropriate chemical treatment (etching). The etching must be isotropic at the zircon grain surface to be used in the FTM, which leads those zircon grains whose etching is anisotropic to be discarded. The only reason for this discarding is the nonuniform morphology of the surface grain seen by optical microscopy, that is, no further physicochemical analysis is performed. In this work, combining micro‐Raman and scanning electron microscopy (SEM) to study the etching anisotropy, it was shown that zircon grains that present at least one area at the surface where the density of fission track is uniform can be used in the FTM. The micro‐Raman showed characteristic spectra of the standard zircon sample either from the areas where there are tracks or from where there are not. The only difference found was in the Raman bandwidths, which were broader for the areas with higher density of fission tracks. This suggests simply a decrease in the relative percentage of the crystalline/amorphous phases at these areas. The SEM/energy dispersive spectrometry (EDX) showed that there were no significant differences in the principal chemical composition at the areas with and without fission tracks. Copyright © 2008 John Wiley & Sons, Ltd.     

Measurement of nanosize etched pits in SiO2 optical fiber conduit using AFM

Fission fragment tracks from ²⁵²Cf have been observed in SiO₂ optical fiber, using an atomic force microscope (AFM), after a very short chemical etching in hydrofluoric acid solution at normal temperature. The nuclear track starting and evolution process is followed by the AFM direct measurements on the material surface and beyond a fine layer of the surface material. The images of the scanned cones were determined observing the two predominant energies from ²⁵²Cf fission fragments and the development of the tracks in the 150 μm diameter optical fiber conduit.     

Observations of fission-tracks in zircons by atomic force microscope

The fission-track (FT) method is a dating technique based on the observation of damage (tracks) by spontaneous fission of ²³⁸U left in a mineral. The date is calculated from the track density and the uranium concentration in the mineral. This is possible because the number of tracks is a function of uranium concentration and time since the start of track accumulation. Usually, the number of tracks is counted under an optical microscope after etching (chemical expansion of a track). However, as FT density per unit area rises, it becomes difficult to count the number of tracks. This is due to the fact that FTs overlap one another and are unable to be readily distinguished. This research examines the potential of atomic force microscope (AFM) for FT dating using zircons, which are likely to show higher FT density than other minerals due to their high U concentrations.To obtain an AFM image for a sample prepared for FT dating, removing the static electricity of the sample is essential to avoid an unexpected movement of the cantilever. A grain should be wider than about 30 μm to bring the cantilever on the mineral surface. Polishing with a fine grained compound is very important. There is not much difference in sharpness between images by AC mode (scanning with vibrating cantilever at a constant cycle) and Contact mode (scanning with the cantilever always in close contact with the surface). To confirm how tracks can be identified with the AFM, an AFM image was compared with an image obtained with the optical microscope. When change in the number of tracks and their shapes were observed through stepwise etching, the track expanded as the etching time increased. In addition, the etching rate was slower for large tracks than those for small tracks. This implied that the AFM can be used to observe etching of zircons with different degrees of nuclear fission damage. A track that could not be seen with the optical microscope due to insufficient etching could be observed by AFM methods, indicating the possibility of FT dating with high track densities using AFM after relatively short etching periods.     

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.     

Chemical etching op fission tracks in ethylene-tetrafluoroethylene copolymer

The chemical etching of fission tracks in ethylene-tetrafluoro-ethylene copolymer was studied. Etched holes 3000–4000 Å in diameter was recognized by electron microscopy for a film bombarded by fission fragments in oxygen and etched in a 12N sodium hydroxide solution at 125°C. The radial etching rate at 125°C was 6–8 Å/hr, which is less than 17 Å/hr for polyvinylidene fluoride in the same sodium hydroxide concentration at 85°C. The smaller rate is a reflection of the larger chemical resistivity of ethylene-tetrafluoro-ethylene copolymer than polyvinylidene fluoride.     

The chemical etching of fission fragment tracks in natural fluorite

An experimental study of the mechanism for chemical etching of fission fragment tracks in the natural mineral fluorite is described. A systematic search showed that a 3:1 mixture by volume of sulphuric to hydrochloric acids was a most appropriate etchant. Experiments directed at determining the etching efficiency as a function of solvent temperature are also discussed. The preferential track etch ratioVt/Vg, the track length and the track density all depend upon the time and temperature of annealing.

It is variations of the fission track density in fluorite, with etching time and annealing temperature, which make possible an overall geophysical interpretation of annealing data for the mineral in terms of the paleoisotherm of its intrinsic fission track clock.

An interactive image analysis system INTIMAN, assembled for the swift and automatic readout of fission fragment track measurements, in both crystalline and non-crystalline materials, is described. Normal procedures for measuring and analyzing tracks are outlined.     

Swelling and structure of radiation induced near-surface damage in CR-39 and its chemical etching

Systematic measurements of swelling of CR-39 nuclear track detector (NTD) due to irradiation with fission fragments and alpha particles over a wide range of fluences from ²⁵²Cf are presented here. Precisely designed and optimized exposure and chemical etching experiments were employed to unfold the structure of radiation induced surface damage. Delays in the startup of the chemical etching of latent tracks in low radiation fluence detectors are measured and are found to contain important information about structure of the surface damage. Simple atomic scale pictures of radiation induced surface damage and its chemical etching are developed using measurements of radiation induced swelling of CR-39 detectors and nuclear track parameters. The computer code SRIM2010 was utilized for the calculations of basic features of latent tracks of fission fragments and alpha particles in CR-39. Another computer code TRACK_VISION was used to compute parameters of etched tracks. Computations and experimental findings in the paper coherently compose a realistic picture of radiation damage.     

Critical etching parameters of mica, Lexan and cellulose acetate track detectors

Chemical etching characteristics of mica, Lexan and cellulose acetate have been studied for fission fragment tracks. Under suitable etching conditions a few critical etching parameters for these three track detectors have been determined. An empirical relationship between complete etching time and the etching temperature has been established.     

Fission studies of gold induced by (1665 MeV) π- using a CR-39 detector

The fission cross section and fission probability of ¹⁹⁷Au, induced by (1665 MeV) π^-, have been studied using CR-39 track detectors. A 4π-geometry was used to count track statistics. A beam of negative pions of 1665 MeV was produced at AGS of Brookhaven National Laboratory, USA, and allowed to fall normally on the stack. Two detectors from the stack were scanned for fission fragment tracks after etching in 6N NaOH at 70℃. The statistics of fission fragment tracks in both detectors were obtained. It was found that there was a marked asymmetry of registered tracks with respect to the forward and backward hemispheres. This asymmetry could be partly accounted for on the basis of momentum transfer to the struck nucleus. On the basis of counting statistics fission cross section was measured, and fission probability was determined by dividing the fission cross section with the reaction cross section. The fission cross-section and fission probability were compared with the computed values using the cascade-exciton model code CEM95.     

Damage morphology of Kr ion tracks in apatite: dependence on dE/dX

With the aim of characterizing damage along nuclear tracks in apatite, Durango fluoroapatite monocrystals were irradiated under a high fluence ⁸⁶Kr ion beam at the G.A.N.I.L. (Grand Accélérateur National d'Ions Lourds, Caen, France). The resulting irradiation damage was studied by associating CRBS spectrometry and chemical etching. By applying Poisson's law to the backscattering results, the nuclear track average effective radius R_e was calculated for different steps along the ion path. On the other hand, the chemical etching experiments allowed us to deduce three different damaging morphologies in correspondence to the R_e values. For the first time in apatite, it has been shown that a defect fragmentation produced along the ion paths may be detected by chemical etching. These results were also applied to fission tracks in order to quantify the damage rate and to describe the damage morphology evolution along fission fragment paths.     

Proton dose-dependent modification in track etching response in some polymers

In the present work, the effect of four different doses of 62 MeV protons, on the fission fragment track etching characteristics of two polymers, viz. polycarbonate (Makrofol-N (MFN)) and polyimide (PI) are studied by nuclear track technique. The bulk etch-rate of PI increased by around 30% at the highest proton dose, whereas the activation energy of etching remained almost constant for the same. A considerable increase in the bulk etch-rate of MFN was observed (75%) at the highest proton dose. The activation energy of etching of the fission fragment tracks in MFN was also found to be an inverse function of dose.     

Etchability of Latent Fission Fragment Tracks in CR-39

We report the chemical etching behaviour of the CR-39 polymer detector exposed to fission fragments of 252Cf describing etchability of latent tracks, which are like nanocylinders. The fission fragment exposed detectors were etched in 1-7 N NaOH water solutions at temperatures 50-80℃ for 45 min in the case of track length and 180 min in the case of track diameter measurements. The reduced etch rate S （called here etchability） is determined using experimental results for all etching conditions and the etching conditions with the highest reduced etch are obtained. Physics and energetics of bulk and track etching are discussed. Possible effects causing spurious changes in determination of activation energy of etching are investigated.     

The influence of etching parameters on the sensitivity of plastics

Abstract

It seems that the critical rate of primary ionization for track registration must also depend on the etching conditions. Simple experimental methods are presented to show a possible change in registration sensitivity as a function of the chemical parameters. It was proved, from investigations of α-particle tracks, that the sensitivity of a cellulose acetate detector can considerably depend on the concentration and type of etching reagent. Quantitative data are given on the ratio of the rate of chemical etching along the track and on the detector surface as a function of concentration of NaOH solution for tracks of fission fragments registered in plastics of cellulose acetate, polycarbonate and polyethylene-terephthalate.     

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.     

Fission studies of gold induced by (1665 MeV) π- using a CR-39 detector

The fission cross section and fission probability of ¹⁹⁷Au, induced by (1665 MeV) π^-, have been studied using CR-39 track detectors. A 4π-geometry was used to count track statistics. A beam of negative pions of 1665 MeV was produced at AGS of Brookhaven National Laboratory, USA, and allowed to fall normally on the stack. Two detectors from the stack were scanned for fission fragment tracks after etching in 6N NaOH at 70℃. The statistics of fission fragment tracks in both detectors were obtained. It was found that there was a marked asymmetry of registered tracks with respect to the forward and backward hemispheres. This asymmetry could be partly accounted for on the basis of momentum transfer to the struck nucleus. On the basis of counting statistics fission cross section was measured, and fission probability was determined by dividing the fission cross section with the reaction cross section. The fission cross-section and fission probability were compared with the computed values using the cascade-exciton model code CEM95.     

A new method for detection of alpha particles in 1 mm thick polycarbonate detectors using 50 Hz – HV ECE method

Recent studies in our laboratory have proved that electrochemical etching (ECE) of polycarbonate track detectors (PCTD) under 50 Hz – high voltage (HV) field conditions has potentials for time-integrated heavy charged particle detection and dosimetry applications. The rationale in the study is the ECE process of alpha particle tracks in 1 mm thick PCTDs by a 50 Hz – HV generator at optimized ECE conditions. Tracks of 3.2 MeV alpha particles from a collimated beam of an ²⁴¹Am source degraded in air and background tracks were registered. The effects of HV and ECE duration on alpha track registration efficiency and track diameters were studied for 3 sets of 50 Hz – 4, 5 and 6 kV field conditions in a PEW solution (potassium hydroxide, ethanol and water) at 26 °C. The optimized ECE conditions obtained at this stage of development for 1 mm thick PCTDs are 50 Hz – 4 kV in PEW solution at 26 °C for 10 h. Alpha track registration efficiency at 3.2 MeV is about 30% with 37 ± 6 μm mean track diameter. The mean background track density at the above stated optimized conditions is about 571 ± 16 tracks.cm⁻² with a mean diameter of 65 ± 5 μm. All tracks are observable by the unaided eyes. The mean background track diameter is near two times larger than that of alpha particle tracks at the optimum conditions applied; they are easily distinguished against each other. This high background track density while at this stage of development seems a drawback for low dose and low fluence particle applications, it has minimal effects on high fluence ion detection applications. The simple 50 Hz – HV generator used proved to be convenient for efficient alpha track amplifications. Studies are underway for improvement of the method in particular for reducing background track density.     

Track revelation and optical properties of pentaerythritol tetrakis (allyl carbonate) plastic for application as nuclear track detector: effects of gamma radiations

The etching conditions of an indigenously prepared thin film of pentaerythritol tetrakis(allyl carbonate) (PETAC) were standardised for the use as a nuclear track detector. The optimum etching times in 6?N NaOH at 70°C for the appearance of fission and alpha tracks recorded in this detector from a ²⁵²Cf solid source were found to be 30 min and 1.50?h, respectively. The experimentally determined values for the bulk and track-etch rates for this detector in 6?N NaOH at 70°C were found to be 1.7?±?0.1 and 88.4?±?10.7?µm/h, respectively. From these results, the important track etching properties such as the critical angle of etching, the sensitivity and the fission track registration efficiency were calculated and compared with the commercially available detectors. The activation energy value for bulk etching calculated by applying Arrhenius equation to the bulk etch rates of the detector determined at different etching temperatures was found to be 0.86?±?0.02?eV. This compares very well with the value of about 1.0?eV reported for most commonly used track detectors. The effects of gamma irradiation on this new detector in the dose range of 200–1000?kGy have also been studied using bulk etch rate technique. The activation energy values for bulk etching calculated from bulk etch rates measurements at different temperatures were found to decrease with the increase in gamma dose indicating scission of the detector due to gamma irradiation. The optical band gap of this detector was also determined using UV–visible spectrometry and the value was found to be 4.37?±?0.05?eV.