"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

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

Institute Ruđer Bošković accelerator facility

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

Research areas

RBS/PIXE/PIGE IAEA beam line

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

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

Heavy ion microprobe with quintuplet focusing Up to ME/q 2 =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,...) 300 nm Heavy ion microprobe

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

T1T1 T2T2 particle detector x,y,z,  manipulator L=52,3 cm chamber for thin film analysis TOF spectrometer at 37.5°, Ω = 0.11 msr, Δt = 170 ps Thin film analysis usingTOF-ERDA

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

Inner shell - X-rays - 1st systematic study of chemical effects in Kβ 2,5 and Kβ’’ x-ray lines in PIXE of transition metals (Ti, V completed, Cr, Mn in progress) Ti V Fazinić et al. Phys.Rev.A, 2006/9 phD thesis, Luka Mandić (Uni Ri.) Study of chemical effects by HR-PIXE

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

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

M. Karlušić et al. New. J. Phys Effects of heavy ion irradiation at nanometer scales 5.3 keV/nm (13 MeV I) 7.2 keV/nm (18 MeV I) 11.3 keV/nm (23 MeV I) 21 keV/nm (92 MeV Xe) 25 keV/nm (700 MeV Xe) Calculations: two temperature model; melting temperature 2353 K; electron-phonon coupling...; result keV/nm - SrTiO 3 - iodine beam - E = 6.5, 13, 18, 23, 28 MeV - φ= AFM Energy threshold for nanodot creation in grazing incidence irr. M. Karlušić, M. Schleberger, et.al

a)as-deposited- no visible clustering CS TEM b) after irradiation- Clustering of Ge atoms and ordering along irradiation direction (c) (d) c) and d) after 1 h annealing in vacuum - transformation of Ge-density fluctuation into well separated Ge QDs QD r = 3.3 ± 0.2 nm - spherical Generation of an ordered Ge QD array in an a-SiO 2 3 MeV O ions

Past PIGE & NRA applications

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

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

HPGe sample 50 µm Kapton 4 MeV p - large solid angle! - multiple scattering in the exit foil (spot size - 80 x 80 μm 2 ) - linear scans of the cross sections of PVdF/HFP samples - I < 100 pA damage! 19 F (p, p’γ) 19 F, E γ = 197 keV 7 Li (p, p’γ) 7 Li, E γ = 478 keV External microbeam PIGE of Li and F distribution in gel polymer batteries

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

HPGe sample 4 MeV p Si(Li) -sample: gel polymer interfaces with Li-anode and spinel (LiMn 2 O 4 )-cathode - in vacuum analysis Microbeam PIGE and PIXE mapping of Li and F distribution in gel polymer batteries Li - PIGE F - PIGE Mn - PIXE T. Tadić, NIMB (2000) 614 T. Tadić, NIMB 181 (2001)404

Microbeam NRA and PIXE on multilayer films designed for optical applications Cladding: SiO 2 (B?) (PECVD) Core: SiO 2 :B 2 O 3 :GeO 2 (flame hydrolisis) Buffer thermal SiO 2 Si Wafer X-ray detector particle detector -PIXE for Si and Ge determination -NRA for B 11 B(p,  ) 8 Be -0.9 MeV protons Samples- Minimum detection limits for 2000 seconds measuring time was about 0.3 at. %. for boron.

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

Use of (d,p) reactions for determination of O in WOx films 16 O(d,p) 17 O 0.85 MeV d mylar =12.8  m standard 6.85·10 17 O on Ta p1p1 p0p0 p1p1 12 C(d,p) 13 C C from the surface sample WO x with 9.7·10 16 O C O /C W varying from 0.02 to 0.15, established correlation between pressure and O concentration

Planned PIGE applications

135° 20%, MeV SB 165° beam FC SB 45° Si(Li) 150° for higher energy x-rays 80 mm 2, keV SDD x-ray detector for low energy X-rays 20 mm 2, keV Use of PIGE in the analysis of aerosol samples

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

10 B 11 B

19 F Eγ=197 keV

23 Na E  =440 keV

24 Mg 25 Mg

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

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° PIGE CRP