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Contents lists available at ScienceDirect

**Applied Radiation and Isotopes
**

journal homepage: www.elsevier.com/locate/apradiso

**A parameterization of the chemistry-normality dependence of bulk etch rate
**

in a CR-39 detector

crossmark

Mushtaq Abed Al-Jubbori

Department of Physics, College of Education for Pure Science, Mosul University, 41001 Mosul, Iraq

A R T I C L E I N F O A BS T RAC T

Keywords: An empirical relationship describing the bulk etch rate is formulated. The equation involves two free ﬁtting

Normality parameters, which reproduce the bulk etch rate for CR-39 by alpha particles at diﬀerent normalities of the

Bulk etch rate etching solution. The values of the ﬁtting parameters were obtained from the experimental data. This

Length–Diameter (L–D) method relationship is used to predict the bulk etch rate at diﬀerent normalities.

Modeling

CR-39

**1. Introduction by the accuracy of mass measurements. The other method used to
**

measure VB is the L–D method, which is based on studying the

Solid state nuclear track detectors (SSNTDs) have applications in relationship between the tracks length L and diameter D for irradiated

nuclear physics, cosmic ray physics, space physics, particle accelerator detectors, and using the relation (Manzoor et al., 2007):

physics, archeology, geology, medicine and biology (Hiroko and

D2 ⎡ 4L2 ⎤

Nobuhito, 2000; Stejny et al., 2000; Rana et al., 2000; Hermsdorf VB = ⎢1 + 1+ ⎥

and Hunger, 2009; Al-Jubbori, 2013). One of the basic parameters 4tL ⎢⎣ D 2 ⎥⎦ (3)

required for the use of an SSNTD is the bulk etch rate, VB (Ditlov et al.,

The use of digital image processing can result in improvement of

2008; Awad et al., 2009; Azooz and Al-Jubbori, 2016). This is deﬁned

measurement accuracies of both methods. Such technique is employed

as the rate at which an etchant erodes the target material in a general

in this work and results from both methods are compared.

direction (Azooz et al., 2012a, 2012b; Hermsdorf, 2012). There are

many methods to determine the bulk etch rate for SSNTDs. The most

2. Experiments

straight forward is the measurement of the eroded thickness, Δh ,

during the etching process of a detector surface in a speciﬁc interval of

For the removed thickness measurement method, unirradiated

time, Δt , then calculating VB (Durrani, 1987) as:

10×10 mm, 200 μm thick CR-39 detectors made by Page Moldings

1 Δh (Pershore, UK). The detector was etched each 10 min, and a digital

VB =

2 Δt (1) image after each etching was obtained and used to obtain the

The factor “2” above takes account of the removal of the thickness remaining detector thickness. Typical image is shown in Fig. 1. The

from both sides of the ﬂat surfaces of a detector sheet. Another method images were analyzed to obtain the remaining detector thickness by

relies on measuring the detector mass before and after etching. Based converting digital pixels to micron thickness. The value of VB following

on the mass diﬀerence and the known density of the detector, it is each etching process was obtained from deﬁning sharp boundaries

possible to determine the thickness of the removed layer and in turn between contrasting picture regions derived from color contours

VB. This method is sometimes called the “gravimetric” method and it calculations.

determine VB (Malik et al.,2002) by: In order to obtain track longitudinal proﬁles and track diameters at

diﬀerent etching chemistry-normality (degree of acidity) and etching

Δm times, detectors were exposed to alpha particles from a 241Am source

VB =

2AρΔt (2) with 3.2 MeV energy. This energy represents the middle of the energy

where Δm is mass diﬀerence, A the etched surface area, ρ the density of range where such detectors are typically used. The exposure system

the detector and Δt is the etching time. However, this method is limited involves narrow collimation in order to obtain an almost perpendicular

E-mail address: mushtaq_phy8@yahoo.com.

**http://dx.doi.org/10.1016/j.apradiso.2016.09.022
**

Received 17 May 2016; Received in revised form 19 September 2016; Accepted 19 September 2016

Available online 20 September 2016

0969-8043/ © 2016 Elsevier Ltd. All rights reserved.

It must be emphasized however that the accuracies of the removed layer results are better than the corresponding L–D method results due to the 0 combined errors in the latter (Hermsdorf et al. Al-Jubbori Applied Radiation and Isotopes 118 (2016) 228–231 Fig. Example of such measurements for the radius is shown in Fig. 8. and digital images for the longitudinal and lateral develop- ment of the tracks were recorded. (b) track diameter at 1 h for E=3.5 3 Jubbori. for track length and diameter..25.9526x -0.3214x -0.25 T=70 C which shows the experimental data and linear ﬁt results at solution y=3. Values of VB Removed Layer Thickness Δ h (μ m) 20 calculated from Eq. track length. The etching process was repeated over several 15 min periods.5 normality of 6.2 MeV. (1).25. B5) attached to OPTIKA B-193 microscope.2589 for N=6. 2(c). Azooz and Al. incidence angle.5. (3) to calculate VB.821x -0.5 in Fig. 3 y=2. was determined for the time-dependent Fig.20661 for N=7. 8. Thickness results from the ﬁrst method discussed above are used to calculate VB using Eq. Results in this ﬁgure indicate that there are no signiﬁcant variations of VB with the exception of those related to the highest normality. The results are presented in Fig. Etching Time (h) The track etch rate.802x -0. while the maximum contour line ﬂuctua- tions amplitude along the contour deﬁned the error in measurement. A special MATLAB image processing software was used to performs image-brightness contour analysis to deﬁne the track boundaries.5 2 2. 3. 3.5 and 9. Typical images are shown in Fig.A.5. The bulk etch rate was determined by 25 o performing a linear ﬁt of Δh versus t.0 N respectively. This quantity can be derived from measured time evolution of the 229 . 1. The detectors are sharply broken at the small 1 mm2 exposed area. y=4.5 and 9. 4. the relationship: VT = dL / dt + VB .0 15 corresponding D values were substituted in Eq. 2(a) and (b). 4(c).M. 2013).5 1 1. Digital images of: (a) track length.7321x -0. It may be worth mentioning here that the track saturation length in Fig. 2. 8. 2007. VT. 0 0. The results related to the time development of VB are presented in Fig.1071 for N=8.4464 for N=8. Relationship between removed layer thickness and etching time. The detector was etched for 10 min and then digitally photographed by a digital USB camera (OPTICA 4083. 8. Digital image of the lateral view of an etched unirradiated detector. (1) are shown in Table 1. L. errors did not exceed 3%. (c) contour edge diameter.359 for N=9. at normality of 6. The outermost well deﬁned contour deﬁned the track dimension.0. Values of L prior to track length saturation together with the y=5. Results and discussions Fig.0 Results of measurements of L and D versus etching time are shown y=4. This gives 5 further credibility to the measurement technique used. 7. respectively. Errors values are aﬀected by image quality. In most cases. 4(a) is independent of etching normality.0 N. The etching was carried out in 70 °C NaOH solutions.0. 7. which suggests a measurement error of about 1%. The 10 time averaged results of all VB values are presented in the third column of Table 1.

which corresponds to inﬁnite track saturation time. a2 = 0. 4. Time development of track dimensions at diﬀerent etching normality: (a) track length. (5) are also compared with two empirical relation proposed by Fromm et al.648 h.828C + 0. (1980) 8 and Ahn and Kilee. This is consistent with the fact that highly concentrated sodium potassium and calcium hydroxides solu.37 ± 0. Any empirical equation that describes 4 the experimental results in Fig. tsat .02 ± 0. The third is that it is also desirable to have an N=9. 4(a)) by calculation of the ﬁrst derivation of L(t). The equation also gives zero bulk etch rate at zero concentration (distilled water).5 and Hunyadi (1979) which described the VB dependence upon both Etching Time (h) concentration C and absolute temperature T in forms: VB = 1.41 ± 0.. and plotted against etching solution normality on Fig. Experimental data and ﬁt results to Eq.00 with a and b as two free ﬁtting parameters. where T is the temperature in K.5 1 1.25 VB = a (e bN − 1) (5) T=70 C N=7. relation to N=8.00 ﬁt. C is the concentration of the etchant in the unit of normality and k is the Boltzmann's constant. E2 )/VB . N=6. (c) bulk etch rate calculated from data in (a) and (b) using Eq.5 VB (μ m/h) tion can vigorously attack most organic materials.25 Fig.5 3 3. 7 must produce numerically acceptable convergent ﬁt in the range of the experimental data considered.478 μm/h .127 + 1.16 ± 0.A.0 2. Al-Jubbori Applied Radiation and Isotopes 118 (2016) 228–231 Table 1 12 Comparison of VB measured in two methods.25 1.50 high concentrations.00 the exponential form in the relationship: 0 0 1 2 3 4 5 6 tsat = a1 e−a2 N + a3 Etching Time (h) (4) The ﬁtting parameters values a1 = 179. this is accepted to be better than any polynomial ﬁt which involves three parameters at least. 6 the results of ﬁt are compared with those of o Hermsdorf and Mahmood (2013).00 Fig. and 12 a3 = 0.0018 h.50 N=8. 2.02 1.5 2 2. the following equation is proposed 3. 2 N=8.90 ± 0.5 o N=6.M.049T − 0.25 N=7. The equation produced 2 the best ﬁt of the data with minimum number of free ﬁtting parameters (two only). (2005). 7.03 3.50 usually an easy task and a polynomial of some degree can result is such 2 N=8. Normality (μm h−1) Bulk Etch Rate VB 10 Removed Thickness Method L–D Method o T=70 C 6.5904 . which corresponds to N=9.50 high bulk etch rate at very high concentration. described the saturation time by T=70 C tsat = (−1. E + 0.0 2. b = 0. The constants 230 .98 ± 0.09 4 track length (Fig. This equation produces very 3 N=8. which usually assumes an exponential behavior. VB = fB C nB e−ε / kT (7) (3).5 2.237. 6 shows the results of track saturation time.09 6 9. 4(a).00 empirical equation with a minimum number of free ﬁtting parameters.00 very small track saturation time. it may be 6 useful to attempt to propose some empirical relationship that properly describes the experimental data. the VB data from this work were combined with other data at a lower normality range published by Gruhn et al. with over 95% conﬁdence level ﬁt. From purely ﬁtting theory point of view.03 2.2151.28 ± 0. 10 In order to develop an empirical relationship between the bulk etch rate and normality. 0 0 1 2 3 4 5 6 Keeping in mind that the reaction between the etching solution and the Etching Time (h) detector material is a ﬁrst-order irreversible chemical reaction.03 2.05 8 7.07 L (μ m) 8.5 parameters above are a = 0. (b) track diameter.244.5 1. In Fig.05 8. These data are well described by N=9.02 1. 5 shows the track etch rate obtained by numerical diﬀerentiation N=7.57 ± 0.50 normality as derived from Fig. In the absence of a detailed theory describing D (μ m) the eﬀect of solution concentration on bulk etching rate. The ﬁtted values of the two 1.50 procedures. This is N=6.002CT − 17. The relationship must also describe the behavior at zero and very N=8.624) (6) Fig.07 ± 0.276 exp(0.80 ± 0. (1991) and Somogyi 1 0 0.

58. D.A. nB = 2.. pp. Track Radiat... A. Weickert. 171–175.00 dependence of VB shown as blue and red dash line in Fig. S.5 process in LR-115 detectors by the many-hit-model. V. Fromm. 443–452. 3. (5)–(7).Li. Lyon. V..A.... M. These corre- 18 N=7.5 Department of Physics.. R...5 Al-Jubbori. F. pp.A. 1 Manzoor. Manzoor. Etching mechanism and present work behavior of polycarbonate in hydroxide solution: Lexan and CR-39. Proton and alpha track proﬁles in Fig. Hermsdorf. Eq. Radiat.. 149–155... Al-Jubbori. 44.. Thermal annealing of Normality ﬁssion fragment radiation damage in CR-39.A. Track saturation time versus normality. Husaini. 163–168. Polymerization structure and track recording is referred to the web version of this article. Hunger. Lyon. Eng. 2012a. Eq(7) type CR-39. 766–774.. the reader Detectors.6414 × 10−5 eV/molecule. 2470–2479. 2.5 Ditlov.V. VT (μ m/h) 10 4. Cozzi. (For interpretation of the references to color in this ﬁgure legend. Meas. 5. J. 5 Fit Hermsdorf and Mahmood 2013 4. Al-Jubbori. B 170. R. Radiat. 2009. 2013. Balestra. Qureshi. 301–305.E.A.Johnson. Alpha particles energy estimation from track diameter 1.N. Interrelated temperature dependence of bulk etch rate and track length saturation time in CR-39 detector. 172. 32. A.. L. 2002..A.HunyadiI. Proc. Technol. Azooz.. Qureshi. A. M.S. N=8. Phys. 0 1 2 3 4 5 6 Etching Time (h) Acknowledgment Fig. Meas. Pergamon Press. Radiat.. VB (μ m h -1) 4 Hermsdorf. Khan. Fromm.H. M. E. B 2 316.M. Al-Nia’emi. 231 . Construction of an environmental radon monitoring system using CR-39 nuclear track detectors. Meas. 0 Suppl. M... Measurements of bulk etch rates for poly-allyl-diclycol carbonate (PADC) and cellulose nitrate in a broad range of concentration and temperature of NaOH etching solution.. M. 44. Determination of track etch rates from wall proﬁles of present equation. 7. Comput.. Bull. Margiotta. Mosul University for useful data discussions. Meas. Interpretationofthebulketching 6 6. CR39 during etching and their implications on track etching models. Al-Nia’emi.00 16 Substitution the temperature value of 70 °C gives the normality N=8. I. Loss Inform. Nucl. M..0318μm/h .0421 and ε / k = 1. 67–72. D. Phys. G.. A. Popa. Hiroko. 1004–1010.. 43. Res.. Karim. Palmer. Starke. Radiat. College of Science. Chambaudet. The results of both methods were in good a agreement. I. 2013. Fig. Meas.. Commun. Malik.A. Radiat. Medinaceli.. 2008... S. 47.. Hunger.. D. Solid State Nuclear Track Detection. 2007. Hermsdorf. Description of the bulk etching rate 3 of CR-39 by an extended Arrhenius-like law in increased intervals of temperature and etchant concentration. A. Appl. W.H. Nucl. Aassim A. Khan.5 development in a CR-39 detector.A. Track etch rate at ﬁve etching solution concentrations. Membrey. It is clear 14 that the result of ﬁt using Eqs.K. Meas. 2005. Saouli.A.E. (5) and (7) produced results which are 12 more consistent with experimental data... 299–305. Khan.. Mahmood. Eq(5) particle tracks etched in direct and reversed direction in PADC CR-39 SSNTDs. F. SomogyiG. H..Cassou. Nucl. 3 Hermsdorf. S82–S86..M.. Awad. K. S.U. 7 Gruhn. These methods are 4 the removed layer method and the L–D method.Eq(6) treatment on the particle registration sensitivity of solid state nuclear track detectors of Somogyi and Hunyodi 1979. 2000. 74–80.H. A.. M. Meas. Al-Jubbori. Radiat. The study of the eﬀect of etching 2 solution concentration on track saturation time indicated an exponen- 0 tial behavior. G. In: Proceedings of the Gruhn et al 1980 10th Conference on SSNTD. 19 (1–4).M. 0. R. Experimental and analytical determination of 4He-ion track development in etched PADC detectors of type CR-39 and its consequences for particle spectroscopy with SSNT detectors. C. 101–106. 1980. Ditlov. which can be described by a simple relationship. D.A. 291– 302. 2016. 1979. Kilee. M. D. V. Grahan values (ﬁlled red circle) and Ahn values at 6 h (ﬁlled blue circle) with results from In: Proceedings of the 10th International Conferenceon Solid State Nuclear Track Eqs.A. J. Instrum.. A parameterization of nuclear track proﬁles in CR-39 detector. 115. Meas. Giacomelli. 518–529... 1991. Awad. Meas. 2013. 6. Instrum.E. 1–7. 395–400. The author would like to thank Prof. E... M. E. (5).J. Empirical parameterization of CR-39 longitudinal track depth. A... Qureshi. M.. E. Methods Phys.. 1987. 2000. Radiat. S... 2012. 2–6 July 1979. E.A. V.5 Azooz. I. Giorgini. J. 2007.. M. 2012b.A. Repo. 2000. Jamil...U. 92–96. Fromm. S. Stejny. 1 Azooz.. E. 7... Comparison of combined VB values from the present work (ﬁlled black squares). 47. Togo. Radiat. Normality Durrani. 2009. Kumar..... 813–820. Carrell. Etching properties of the CR-39 polymer nuclear track detector.5 References Track Saturation Time (h) 4 Ahn.Benton.K. Azooz of the 5. Eﬀ. M. S. Nucl. Defects Solids 168 (11–12). Swelling in CR-39 and its eﬀect on bulk etch-rate. Res. 5 Hermsdorf. Al-Jubbori Applied Radiation and Isotopes 118 (2016) 228–231 20 fB . M. I.A. Pergamon Press.50 spond to activation energy of 8. Nuclear track detectors for environmental studies and radiation monitoring. M. Change in the sensitivity of CR-39 for alpha-tracks after storage 2 at diﬀerent temperatures. Radiat. M. Errico.5 8 8. Dr.50 N=9.. Radiat. M. Nucl.25 dures as fB = 0. 42.A.5 9 9. F. S. Patrizii. 37 (4). A. Conclusions 8 The use of digital image processing to study the bulk etch rate of 6 CR-39 nuclear track detector resulted in improved accuracy in measur- VT=VB ing this quantity using two well-known methods. New York. Methods Phys..5 7 7. E.. Sajid. Azooz. S. Oxford. Extension of alpha particles in CR-39-etched track depth model to heavier ions. 183.) properties of CR-39 cured with UV photoinitiators. 35. Nobuhito.. 6 Ahn and Kilee 2005 Hermsdorf. Inﬂuence of external and internal conditions of detector sample Fromm et al 1991. Isot. T. 1–7.M.. D. S. nB and the activation energy ε were obtained from ﬁtting proce- T=70 oC N=6.. 3 4 5 6 7 8 9 10 11 12 13 Rana. Al-Jubbori.. Radiat..0019 K.

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