"Past and planned PIGE applications at the Ruđer Bošković Institute in Zagreb"

1. "Past and planned PIGE applications at the Ruđer Bošković Institute in Zagreb" Iva Bogdanović Radović Laboratory for Ion Beam Interactions Ruđer Bošković Institute Zagreb, Croatia dr. Milko Jakšić dr. Zdravko Siketić dr. Tonči Tadić Ivana Zamboni, BSc

2. Outline • Institute Ruđer Bošković accelerator facility • Research areas • Past PIGE & NRA applications • PIGE for aerosol analysis

3. Institute Ruđer Bošković accelerator facility

4. Duoplasmatron Tandetron Sputtering EN Tandem Van de Graaff Alphatross RBI Accelerator Facility Air pollution beam line External beam Dual beam chamber PIXE RBS H.R. PIXE H.R. ERDA Nuclear microprobe Nuclear reactions

5. Research areas

6. RBS/PIXE/PIGE IAEA beam line

7. Air pollution beam line TC IAEA Project CRO8008: „Upgrades of nuclear analysis techniques for air pollution monitoring”

8. Dual beam chamber • Simultaneous implantation of two ions • Simultaneous irradiation & analysis Couple of weeks ago first test RBS channeling spectra!

9. 300 nm Heavy ion microprobe • Heavy ion microprobe with quintuplet focusing • Up to ME/q2=20 MeV, minimum spot size 300 nm • All IBA techniques (PIXE, RBS, NRA, ERDA, STIM, IBIC) • Unique features (IEE ERDA, coincident scatt., hit detection, tomography,...)

10. Cultural heritage applications-external & microbeam Example: Apoxiomenos D. Mudronja et al. J. Arch. Sci. 2010

11. Thin film analysis usingTOF-ERDA x,y,z, manipulator T2 T1 L=52,3 cm chamber for thin film analysis particle detector TOF spectrometer at37.5°, Ω= 0.11 msr, Δt= 170 ps

12. surface Ti surface Al N 20 nm AlN/TiN multilayer 25 MeV I surface

13. Study of chemical effects by HR-PIXE • Inner shell - X-rays • 1st systematic study of chemical effects in Kβ2,5 and Kβ’’ x-ray lines in PIXE of transition metals (Ti, V completed, Cr, Mn in progress) Ti Fazinić et al. Phys.Rev.A, 2006/9 phD thesis, Luka Mandić (Uni Ri.) V

14. Non-Rutherford cross sections Non-Rutherford cross sections (p,p), (a,a) IAEA CRP project ‘Development of the cross section data base’ ERDA CS 1H(7Li,1H)7Li I.Bogdanović Radović et al. J.Appl. Phys 2009 Z. Siketić et al., NIM B229 (2005) 180 – 186

15. Ion beam modification Cl ions (dE) (dx)el (dE) (dx)nucl protons (dE) (dx)el (dE) (dx)nucl

16. Effects of heavy ion irradiation at nanometer scales Energy threshold for nanodot creation in grazing incidence irr. M. Karlušić, M. Schleberger, et.al 5.3 keV/nm (13 MeV I) 7.2 keV/nm (18 MeV I) 11.3 keV/nm (23 MeV I) • Calculations: two temperature model; melting temperature 2353 K; electron-phonon coupling...; • result - 12.5 keV/nm • - SrTiO3 • iodine beam • E = 6.5, 13, 18, 23, 28 MeV • φ=1.30 • AFM 25 keV/nm (700 MeV Xe) 21 keV/nm (92 MeV Xe) M. Karlušić et al. New. J. Phys. 2010

17. Generation of an ordered Ge QD array in an a-SiO2 3 MeV O ions CS TEM b) after irradiation- Clustering of Ge atoms and ordering along irradiation direction • as-deposited- no • visible clustering (d) (c) QD r = 3.3 ± 0.2 nm - spherical c) and d) after 1 h annealing in vacuum - transformation of Ge-density fluctuation into well separated Ge QDs

18. Past PIGE & NRA applications

19. X-ray and γ-ray spectroscopy of coal and coal ash samples Use of XRF, PIXE and PIGE for characterization of coal and coal ash samples, both on thick and thin samples 28Si(p,p’γ) Eγ=1779 keV 12Ci(p,p’γ) Eγ=4439 keV PIGE for Li, C, F, Na, Mg, Al and Si O. Valković et al, NIM B69 (1992) 479 A. Caridi et al., NIMB66 (1992)298

20. Thick target yields were measured for: 19F(p,p’γ)19F Eγ = 197 keV Ep= 2.3 – 3.3 MeV 23Na(p,p’γ)23Na Eγ = 440 keV Ep=2.3 – 3.5 MeV 23Na(p,αγ)23Na Eγ = 1634 keV Ep=2.3 – 3.5 MeV 28Si(p,p’γ)28Si Eγ = 1779 keV Ep=2.8 – 5.0 MeV

21. - large solid angle! - multiple scattering in the exit foil (spot size - 80 x 80μm2) - linear scans of the cross sections of PVdF/HFP samples - I < 100 pA damage! 19F (p, p’γ) 19F, Eγ = 197 keV 7Li (p, p’γ) 7Li, Eγ = 478 keV External microbeam PIGE of Li and F distribution in gel polymer batteries HPGe 4 MeV p sample 50 µm Kapton

22. Li γ-ray - distribution of Li+ ions within the gel polymer F γ-ray - homogeneity of the gel polymer

23. Li - PIGE Mn - PIXE F - PIGE T. Tadić, NIMB 161-163 (2000) 614 T. Tadić, NIMB 181 (2001)404 Microbeam PIGE and PIXE mapping of Li and F distribution in gel polymer batteries Si(Li) HPGe 4 MeV p sample • sample: gel polymer interfaces • with Li-anode and spinel • (LiMn2O4)-cathode • - in vacuum analysis

24. Microbeam NRA and PIXE on multilayer films designed for optical applications particle detector Cladding: SiO2 (B?) (PECVD) Core: SiO2:B2O3:GeO2 (flame hydrolisis) Buffer thermal SiO2 Si Wafer X-ray detector • PIXE for Si and Ge determination • NRA for B 11B(p,)8Be • 0.9 MeV protons Samples- Minimum detection limits for 2000 seconds measuring time was about 0.3 at. %. for boron.

25. O (RBS) Si (RBS) particle spectrum protons, 0.9 MeV 11B(p,)8Be Ge (RBS) Si (PIXE) B (NRA) Ge (PIXE) B (NRA) Si K x-ray spectrum protons, 0.9 MeV Ge L Ge K Full horizontal scale ~ 90 mm

26. Use of (d,p) reactions for determination of O in WOx films 16O(d,p)17O 0.85 MeV d mylar =12.8 m standard 6.85·1017 O on Ta p1 p0 12C(d,p)13C C from the surface sample WOx with 9.7·1016 O p1 CO/CW varying from 0.02 to 0.15, established correlation between pressure and O concentration

27. Planned PIGE applications

28. Use of PIGE in the analysis of aerosol samples Si(Li) detector @ 150° for higher energy x-rays 80 mm2, 155 eV @ 5.9 keV SB detector @ 165° beam HPGe @ 135° 20%, 2 keV @ 1.33 MeV SDD x-ray detector for low energy X-rays 20 mm2, 135 eV @ 5.9 keV FC SB detector @ 45°

29. PIGE for analysis of light elements for new air pollution beam line • Li, B, F, Mg, Na, Al • - γ-ray absorption negligible but γ-ray cross sections strongly • depends on Ep • energy loss of p in the aerosol sample depends on particle size and is • For PM10 and 2 MeV protons ≤ 150 keV • it is important to find regions in the cross section where excitation • function is nearly constant • yield measurements for elements where no data are available around • 2 MeV • - Micromatter standards

30. 10B 11B

31. 19F Eγ=197 keV

32. 23Na Eg=440 keV

33. 24Mg 25Mg

34. 27Al 27Al(p,p’γ)27Al(Eγ = 843 and 1013 keV)

35. PIGE CRP What is the applicability of using PIGE with 2 MeV protons? - measurements of PIGE differential cross sections for light elements. - for that purpose, thin targets evaporated on self supporting C foils will be used - for the normalization purposes, thin Au layer will be evaporated on the top of the target - measurements will be done together with RBS measurements at 165°