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IBA from an old U-120 Cyclotron to a new 3 MV TANDETRON- a Real Challenge

Dorin Dudu, Ofelia Muresan, Herman Schubert, Ion Vata DFNA-Cyclotron NIPNE. IBA from an old U-120 Cyclotron to a new 3 MV TANDETRON- a Real Challenge. (New Experiments and ideas for the 3 MV TANDETRON ). Long-term Goal. New, modern R&D vision in Surface Sciences and Technology by:

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IBA from an old U-120 Cyclotron to a new 3 MV TANDETRON- a Real Challenge

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  1. Dorin Dudu, Ofelia Muresan, Herman Schubert, Ion Vata DFNA-Cyclotron NIPNE IBA from an old U-120 Cyclotron to a new 3 MV TANDETRON- a Real Challenge (New Experiments and ideas for the 3 MV TANDETRON )

  2. Long-term Goal • New, modern R&D vision in Surface Sciences and Technology by: • New basic and applied researches in Astrophysics, Life, Environment ,Earth, Archaeology Sciences and last but not least Industry/Technology • New approach in using Ion Beams in characterization of nanostructured materials • On line and off line measurements of the modifications produced by irradiation • Increase the national/international attractiveness and visibility of our Institute, offering the 3 MV Tandetron as a interesting R&D infrastructure • Development certified analytical services using nuclear methods: • Cheaper analysis • More customers and users • Increase beam time (the degree of occupation) • Improve the economical efficiency

  3. Customers and Users • There are two kind of customers and users: • Local customers and users and external customers and users • Local customers and users: - are familiarized with the IBA experiments - have not possibilities to prepare “interesting” samples • The external customers and users are not very well familiarized with IBA methods but THEY are preparing samples and being interested in characterization of the results of applied technologies • The “parts” must be interested in collaboration

  4. Customer needs/requirements • We cooperated with scientists involved in nanotechnologies and new material discovery/ production and we observed that they are interesting for: • Chemical stoichiometry samples • Element identification • Layered samples structures (depth profile): - order and thickness, in μm-nm range; - chemical composition; - interfaces resulted as effect of the diffusion, migration or implantation of some ions) • To not deteriorates the samples • To have comparative studies on the same sample • To identify the effect of technological procedures ( thermal annealing, etc)

  5. Exemples of Fulfilling Customer Needs at U-120 Cyclotron • We implemented a dedicated infrastructure for RBS at U-120 Cyclotron and methods aiming to enlarge the analytical possibilities: • STOICHIOMETRY (composition) determination - Materials with form memory - Optical fiber • Thickness of layers measurements -Hard nano-structured coatings (superlattices) - Structured thin deposition possible to be used in fusion experiments - Thin magnetic material ( spin valves) - Thin and thick PZT or BZT amorphous composites • Depth profiling of composition - Implanted samples - Interfaces at the borders of different layers

  6. Implementation of a dedicated infrastructure for IBA at U-120 Cyclotron • Accelerated beams at U-120 Cyclotron for IBA • Beam line and reaction chamber (End station) with spectroscopic chains and acquisition data system • Dedicated software for experimental data processing and simulations and etalons and references used for checks and calibration

  7. Accelerated beams at U-120 Cyclotron for IBA

  8. Beam line and reaction chamber -Old Ortec and new NEC RC41 End station for IBA Five axes goniometer • Micron deplacement • Minutes rotation • Many samples holder system and canal lock • PC based application for movement, acquisition and data analysis

  9. Dedicated software for experimental data processing/simulations and etalons/reference samples Thin radioactive source of 238Pu241Am for calibration of SSB detector and spectroscopic chain Cr Au Si > 300μm 100nm 16nm SIMNRA software for analyzing samples

  10. Dedicated software for experimental data processing/simulations and etalons/reference samples Certified etalon of 5+4 alternative layers of 56 nm Cr and Ni, having the same thickness of layers with 2% precision, deposited on Si [Red: experimental data, Blue: simulated data for deduced parameters.]

  11. Concern for infrastructure and methods developments aiming to enlarge the analytical possibilities In order to extend the field of IBA’s, we have been looking for possibilities to achieve micro beams with our cyclotron introducing a conical glass capillary (up left) into the beam line, we could achieve micro beams with reasonable intensities and acceptable quality (Energy spread, divergence etc.). • Analyzing the RBS spectra of a 50nm gold foil on Al with and without glass capillary substrate results than: • -initial energy and energy dispersion is conserved; • -app. 15% of the output beam has an energy loss or energy degradation from the initial energy going at energies of less than 100keV

  12. P2 (P1 după tratament) C Ni O O Nb Ti C • STOICHIOMETRY (composition) determinationused as technological support - materials with form memory - NRA analysis of the sample before and after a thermal annealing shows a strong (app. 300nm) migration of C (contaminant) below the surface.

  13. STOICHIOMETRY (composition) determination-optical fiber with microbeam- Stoichiometry measurement Microbeam

  14. Strat de aderenţă 5x2straturi Zr(C)N/Ti(C)N Si (substrat) Ti d2 d1 ~300μm ~400nm RBS cu N la 3MeV pentru proba P3 30o ZrN ZrCN ZrN ZrCN TiN TiCN TiN TiCN Thickness of layers measurements Measurement of the layers thickness fornano-layered samples : d1, d2 =15-20nm using ionsof He and N 45o 65o

  15. Thickness of layers measurements-spin valves- Using the simulating program SIMNRA vs. 6.05, the following structure for (a) was obtained: Mo0,9O0,1/Fe0,25Co0,35O0,4 /Cu1,0/ Fe0,30 Co0,65O0,05 /Fe0,25Mn0,75/ Mo0.9 O0.1/Si0,33 O0,67on Si substrate with the corresponding layer thicknesses: 4[nm]/5,5[nm]/12,2[nm] /6[nm]/18[nm]/10[nm]/32[nm]/∞ By the same procedure, the elemental composition for (b) was established as: Mo0,9O0,1/Fe0,5Co0,5/Cu1,0/Fe0,4 Co0,6/Fe0,7Mn0,3/ Cu0,9O0,1on Si substrate with the thicknesses of the layers being: 3[nm]/4[nm]/6[nm]/14[nm]/15[nm]/7[nm]/ ∞

  16. Element identification-sample containing N, O, Si,Ti,Zr,Ag,Ir-

  17. Depth profiling of element concentration-Oxygen implanted in Si- Depth profiling of implanted O in Si before and after thermal annealing shows a 50nm migration of O layer toward inside of bulk Si

  18. Depth profiling of element concentration-interfaces structures- A B Buffer layer Pt100nm /Ti20nm /Si A) Sample as deposited B) PtTiSi interface after annealing at 800oC

  19. Depth profiling of element concentration-interfaces structures- Ti on Si deposition by magnetron sputtering (buffer layer) analysis: • RBSspectrum shows an non uniform concentration of deposited Ti layer. For a good fit with simulated spectrum, was necessary to involve 4 sublayers of TiNO of app. 68nm thickness with different stoichiometry. • This result suggest the influence of residual gases inside deposition chamber which are combining with Ti ions from produced plasma.

  20. New Fields and new possible experiments/applications at the 3 MeV tandetron

  21. New possible experiments/applications at the 3 MV tandetron • Channeling of ions into crystalline structures is a powerful tool to inspect the disorder in crystals as well as to find and locate the position of impurities in crystals. Also, in crystalline heavy matrices, channeling technique allow the measurement of light elements (C, O, N) impurities • Complex simultaneously/successive IBA methods aiming a better characterization of a large class of samples (RBS, PIXE, PIGE, NRA, HIRBS). • Microbeam scanning of surface micro-structured samples:

  22. New possible experiments/applications at the 3.5MeV tandetron • Studies of beams scattering at large grazing angles on amorphous and crystalline samples (studies of phenomenon which occur in focusing effect of tapered glass capillaries and so called “surface channeling of ions”). In this way it is possible to obtain in a simple way “nano-beams” for analytical applications. • The existing beam line dedicated for implantation of ions in solid open exciting ways for collaborative R&D applications: • - nanocavities layers induced by different ions ions implanted in semiconductors acting as getter for metallic impurities and silicon nanocrystals embedded in silicon dioxide which exhibit a strong room temperature luminiscence XTEM images showing the microstructure and disorder around bubbles and nanocavities in Si following 100 keV H implantation to a dose of 3x1016 cm-2 and annealing to a) 500oC and b) 750oC. a) RBS Au profiles both as-implanted and after 850oC annealing for an 8x1014 Au cm-2 implant into Si that has a cavity band at a depth of 1μm. b) An XTEM micrograph of the cavity band region after annealing.

  23. Ion irradiation for cell surgery with glass capillaryY. Iwai et al., Appl. Phys. Lett. 92 023509 (2008).

  24. Strengths and Advantages • Very good parameters of the accelerated beams (energy stability and resolution, micro beam facility), easy handling (computer controlled of the accelerator and beam transport) • Possible use of simultaneous methods (RBS, PIXE, NRA, PIGE) • Large number of ion species being accelerated • Dedicated beam line for complex Ion Beam Analysis • Dedicated beam line for ion implantation • Existing experience in IBA applications at IFIN-HH • Important national/international teams involved in material sciences can have benefits of this R&D infrastructure for IBA as a powerful tool for more complete characterization of sample as composition and structure

  25. Thank You for Your attention

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