Wear Measurements By Means Of Radioactive Ion Implantation. L. Gialanella, G. Imbriani, V. Roca, M. Romano Dipartimento di Fisica, Università di Napoli “Federico II” and INFN Naples, Naples,Italy N. De Cesare, A. D’Onofrio, F. Terrasi Facoltà di Scienze Ambientali, Seconda Università di Napoli and INFN Naples, Naples,Italy H. W. Becker, D. Rogalla, A. Stephan, F. Strieder Institut fuer Experimentalphysik III, Ruhr Universitaet Bochum, Bochum, Germany Z. Fulop, G. Gyurky, E. Somorjai Institute of Nuclear Research (ATOMKI), Debrecen, Hungary M. Russo Dipartimento di Ingegneria dei Materiali per l’Energetica, Università di Napoli “Federico II”, Naples,Italy D. Daliento, N. Sanseverino Dipartimento di Ingegneria Elettronica e delle Telecomunicazioni, Università di Napoli “Federico II”, Naples,Italy Abstract. Radioactive ion implantation allows non-contacting, online wear measurements with sub micrometric sensitivity to be performed, by monitoring the removed and/or residual activity on parts subject to wear. Comparative studies of different materials, including those who exhibit a low resistance to radiation damage, can be easily performed by means of this technique. A project has started at the TTT3 tandem of the University “Federico II” in Naples, Italy, in order to exploit such technique using a 7Be ion beam, that was developed to study the astrophysical important reaction 7 Be(p,γ)8B. The 7Be ion beam is produced using a ion sputter source and accelerated to an energy up to 8.0 MeV. A novel setup allows control of the implanted ion depth distribution, and is a crucial point for the application of this technique. The 7Be ion beam production and implantation procedures are discussed. Finally, the results of some test measurements are presented. CP680, Application of Accelerators in Research and Industry: 17th Int'l. Conference, edited by J. L. Duggan and I. L. Morgan © 2003 American Institute of Physics 0-7354-0149-7/03/$20.00 469 the radioactive ion beam production easier in respect to the case of short lived nuclides, that necessarily need an on line production and acceleration. A good case is 7Be (T1/2=53 d), that decays by electron capture to 7Li, with a probability of about 10% by emitting a γray (Eγ=478 keV), corresponding to the population of the first excited state in 7Li. At the 3MV tandem accelerator of the University of Naples Federico II a 7Be beam was developed to investigate the astrophysical important reaction 7 Be(p,γ)8B. Here we report about the results of a preliminary study about its possible use for wear measurements and, in particular, about a novel ion beam energy degrader, which allows a continuous variation of the ion beam energy during the implantation. INTRODUCTION Radioactive tracer techniques are nowadays routinely used for non contacting, on line wear and corrosion measurements and represent an extremely powerful tool in material science and engineering. Indeed, they provide accurate and real-time data, monitoring wear or corrosion without disassembly and physical inspection. The basic principle is to incorporate radioisotopes (preferably γ-ray emitters) in the sample to be tested and to monitor the loss of material due to wear or corrosion by measuring the resulting decrease of the residual activity or, in a complementary way, the increase of the radioactivity accumulated in the lubricant fluid. A basic requirement is an accurate knowledge of the density distribution of the radioisotopes in the direction in which the wear proceeds, in order to infer the wear parameters from the observed variations of radioactivity. Presently, two radioactive tracer techniques are typically used: bulk activation (BA) and surface-layer activation (SLA). In both cases, radio-isotopes are produced directly in the sample by irradiating it with neutrons, for BA, or light charged particles (protons, deuterons and alphas), for SLA. A common problem of these techniques is that their application depends on the material to be tested and it is limited to those materials that exhibit a high activation cross section and, in particular in the case of SLA, strong resistance to radiation damage. Moreover, the radio-isotope depth distribution is governed by the energy dependence of the activation cross section, that strongly limits the possibility of optimising it in view of specific requirements of the test. Radioactive ion implantation (RII) was suggested as a possible solution to such problems [1,2, and references therein]. In this approach a radioactive ion beam (RIB) is used to implant radio-isotopes in the surface layer of the sample. The implantation depth is determined by the beam energy and the stopping power of the radioactive ion in the sample: therefore a proper modulation of the ion beam energy during the implantation in a given material allows a quite wide range of possible radio-isotope depth distributions. The drastic reduction of the radiation damage (up to a factor 106) in comparison with SLA allows application of RII in principle to any material, therefore providing a powerful tool for comparative studies. The main problem of this technique is the availability of a suitable RIB. As in the case of activation techniques, half lives of the same order of magnitude as the duration of the tests, typically some weeks, are preferable, in order to minimize the amount of activity needed to achieve the required sensitivity. This makes 7 Be ION BEAM PRODUCTION Details about the 7Be ion beam production have been reported elsewhere [3]. Shortly, 7Be is produced via the 7Li(p,n)7Be reaction using a 11 MeV proton beam on a 7Li metallic target. Then 7Be is chemically extracted from the 7Li matrix and put in form of 7BeO in a cathode of a sputter ion source, whose average activity is 10 GBq. The ion source delivers a 23 keV 7 BeO- beam, which is injected into the tandem accelerator, together with an accompanying 7LiObeam, originating from the residual Li in the cathode. The interaction with the carbon stripper foil in the terminal, breaks the 7Be and 7LiO molecules and the resulting 7Be and 7Li ions emerge from the accelerator in all their possible charge states, with the corresponding energies. The beam of interest, 7Be3+ E=8.0 MeV, is selected by means of a 90° analysing magnet. Actually, in order to filter out the 8.0 MeV 7 3+ Li contamination, a post stripper carbon foil is used to form the 7Be4+ at 8 MeV before the analysing magnet. Using cathodes of about 10 GBq, typical beam intensities are of several ppA over some tens of hours. This corresponds to a ratio between the total number of 7Be ions obtained from the integrated current after the analysing magnet and the number of ions available in the cathode of the order of 6 · 10-5, i.e. about 0.6 MBq of 7Be are available for implantation. It should be pointed out that for those applications in which a Li contamination of about 50% and somewhat lower beam energy is acceptable, e.g. 5 MeV, the amount of 7Be could be increased by a factor of 5. 470 7 equation 1 it is assumed that the wear proceeds along the z direction and dz/dt represents the wear speed, while dN/dz is the radio-nuclide depth distribution, that, in the case of ion implantation, is given by the following formula: BE ION IMPLANTATION As already mentioned, a crucial point in radioactive tracer techniques is an accurate knowledge of the distribution of the radio-isotopes. Indeed, if A is the observed activity on the sample at the time t, corrected for radioactive decay, then its variation due to loss of material is given by: dA/dt=ε⋅dN/dz⋅dz/dt dN/dz = ∫dN/dE⋅f(z ;E) dE where E is the ion beam energy, f(z;E) is the implantation depth distribution for a monoenergetic ion beam with energy E, and dN/dE is the radioactive ion beam energy distribution. (1) where ε includes the detection efficiency and the eventual branching to non detectable transitions: in 50 mm 40 mm gas outlet mylar foil =10 mm φ 7 gold coated mylar foil φ =8 mm Si 2 Be ion beam target Si 1 pressure transducer pressure read pressure control unit set valve (2) gas inlet solenoid valve MCA1 MCA2 SCA1 SCA2 LOG FILE (P,t,Nel1,Nel2) set (P,t,Nel1,Nel2) read Ar gas bottle set pressure computer read pressure implantation profile parameters a0,..,a8 energy loss data b0,..,b4 FIGURE 1. Schematic representation of the implantation setup. See text for details. 471 Therefore a proper modulation of the beam energy allows to tailor the implantation profile to match specific requirements of the measurement, within the limits set by the range fluctuations for a given incident beam energy, i.e. f(z;E). This can be accomplished setting the highest necessary beam energy and degrading it by means of a gas absorber. The main advantage of this technique is a drastic reduction of the time required for tuning the beam and the possibility of a continuous variation of the beam energy. On the other hand, the ion beam quality is worsened by the energy and angular straggling in the absorber. In this approach, one gets the following expression for dN/dE: dN/dE=∫dN/dP⋅g(P ;E)dP system by means of an interface (National PC1024). The pressure ramp is determined in order to obtained the desired implantation depth profile dN/dz, which has to be provided in form of polynomial, taking into account the energy loss data and range data, which are again provided in form of polynomials. The beam current, and therefore the amount of ions implanted, and energy are monitored on-line as a function of the gas pressure by means of two silicon detectors, that detect the 7Be ions elastically scattered at 45° by a thin Au layer deposited on the outer surface of the exit window of the gas cell. The signals from the detectors are split and sent to two multichannel analysers, to observe the energy spectra of the detected particles, and two single channel analysers, which generate a logic signal and send it to the control computer. The number of detected ions at a given pressure, corrected for the energy dependence of the elastic scattering cross section, is proportional to the number of ions impinging on the target at the corresponding energy, i.e. to the number of ions implanted at the depth corresponding to their range. Figure 2 shows the results of a test implantation performed on a stack of Ni foils (thickness 0.25 µm), where we intended to obtain an implantation profile linearly decreasing with the depth. The number of ion implanted on each foil was determined detecting the γ-rays originating from their decay using a high purity Germanium detector. The overall agreement is good, except for the first foils. This is due to the fact that the maximum pressure in the gas absorber reached during the test was limited to 250 mbar, in order to keep the energy of the scattered 7Be ions at 45° above the threshold of the silicon detectors used for monitoring the beam current. (3) where g(P;E) represents the energy distribution of the ion beam energy with incident energy E0 after passing through the gas absorber at pressure P. The weight function dN/dP is determined by the modulation of the gas pressure in the absorber during implantation. It is clear that a proper variation of the pressure in the gas absorber produces the desired implantation profile. On the basis of these considerations, a novel implantation set-up has been realized, which is shown schematically in figure 1. Shortly, the beam passes through a gas absorber and hits the target: the absorber consists of a 8 N (4x109 ion/µm) 7 experimental 6 5 expected 4 3 CONCLUSIONS 2 1 Direct implantation of 7Be ions provides a tool for sub micrometric, non-contacting, on-line wear measurements that can be used also for those materials, e.g. polymers, for which the presently available radioactive tracer techniques cannot be applied. The control of the implantation depth profile is a crucial point for this technique. An implantation set-up has been realized and tested, that uses a gas absorber in order to obtain a wide variety of implantation depth profiles by a proper variation of the gas pressure in the absorber. The first results of a test measurement show a fair agreement between the measured implantation depth profile and the expected one. Further work is in progress to improve this technique and extend its use to other fields of ion implantation, where also implantation profile tailoring 0 0 1 2 3 4 depth (µm) FIGURE 2. Result of a test implantation of 7Be ions on a stack of Ni foils. See text for details. gas cell: the total energy loss in the absorber is given by the energy loss in the entrance and exit windows of the cell (mylar, thickness 2 µm) plus the energy loss in the gas (Ar, l=50 mm, p=0-500 mbar). The pressure in the gas cell is regulated by a system composed of a capacitance manometer (MKS, mod 626A), a control unit (MKS250E) and an electromagnetic valve (MKS, mod 248). The pressure set point is provided by a computer, which is connected with the pressure control 472 is needed. In particular, a program has started to exploit the advantages of implantation profile tailoring in lifetime engineering processes, needed in power electronics devices, able to modify in a selective way the value of the recombination lifetime in semiconductor materials. ACKNOWLEDGEMENTS The authors thank L. Campajola of the Università di Napoli Federico II, Naples, for his help during the beam time at the tandem accelerator in Naples and M.Roth, and the staff at the Isotop-Labor of the RuhrUniversitaet Bochum for their help during the preparation of the 7Be cathodes. We also thank L.Ando and the staff at the cyclotron of Atomki, Debrecen, for the production of 7Be. REFERENCES 1. McHarris,Wm.C. et al., Nucl. Instr. and Meth.A 353, 583-587 (1994). 2. Fehsenfeld, P. et al., Nucl. Phys.A 701, 235c-239c (2002). 3. Gialanella, L. et al., NIMB 65, in press 473
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