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

Iva Bogdanović RadovićLaboratory for Ion Beam Interactions

Ruđer Bošković InstituteZagreb, Croatia

dr. Milko Jakšićdr. Zdravko Siketićdr. Tonči TadićIvana Zamboni, BSc

• Institute Ruđer Bošković accelerator facility

• Research areas

• Past PIGE & NRA applications

• PIGE for aerosol analysis

Outline

Institute Ruđer Boškovićaccelerator facility

Alphatross

SputteringDuoplasmatron

Nuclearmicroprobe

H.R. PIXE

Nuclear reactions

H.R. ERDA

PIXERBS

EN Tandem Van de GraaffTandetron

External beam

RBI AcceleratorFacility

S1

S2

M1

M2

M3

D1D2 Q1

tQ2

Q3

QM

DM

E1E2

HV

F1F2

F3

F3

tQ1 tS2 tM2

tM3

S3

tM1

F1tS1

tE1 tL1

tHV

tS1

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/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,...)

300 nmHeavy ion microprobe

Example: Apoxiomenos

D. Mudronja et al. J. Arch. Sci. 2010

Cultural heritage applications-external & microbeam

T1T2

particle

detector

x,y,z,manipulator

L=52,3 cm

chamber forthin 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

Alsurface

Tisurface

N

surface

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

V

Fazinić et al. Phys.Rev.A, 2006/9phD 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 1H(7Li,1H)7Li

Z. Siketić et al., NIM B229 (2005) 180 – 186

10 100 1000 10000 1000000.01

0.1

1

10

100

1000

10000

Ene

rgy

loss

(eV

/nm

)Energy (keV)

(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. 2010

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 - 12.5 keV/nm

- SrTiO3

- iodine beam- E = 6.5, 13, 18, 23, 28 MeV - φ=1.30

- AFM

Energy threshold for nanodot creation in grazing incidence irr.M. Karlušić, M. Schleberger, et.al

a) as-deposited- novisible 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 - transformationof 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-SiO2 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:

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

HPGe

sample

50 µm Kapton

4 MeV p- large solid angle!- multiple scattering in the exit foil (spot size - 80 x 80 μm2)

- 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 ingel polymer batteries

20 30 40 50 60 70 80 90 100 110 1200

50

100

150

200

250

Liimide 4 Li478 F197

Yiel

d

Channels

30 40 50 60 70 80 90 100 110 1200

50

100

150

200

Libeti 2 Li478 F197

Yie

ld

Channels

30 40 50 60 70 80 90 100 110 1200

50

100

150

200

250

300

350

Libeti 3 Li478 F197

Yiel

d

Channels

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

HPGe

sample

4 MeV p

Si(Li)

-sample: gel polymer interfaces with Li-anode and spinel (LiMn2O4)-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 161-163 (2000) 614T. Tadić, NIMB 181 (2001)404

Microbeam NRA and PIXE on multilayer films designed for optical applications

Cladding: SiO2 (B?) (PECVD)Core: SiO2:B2O3:GeO2 (flame hydrolisis)Buffer thermal SiO2

Si WaferX-ray detector

particle 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.

O (RBS)

Si (RBS)

Ge (RBS)

B (NRA)

particle spectrumprotons, 0.9 MeV11B(p,)8Be

x-ray spectrumprotons, 0.9 MeV

Ge K

Ge LSi K

SILICON

BORON

A B C

B (NRA)

Si (PIXE)

Ge (PIXE)

Full horizontal scale ~ 90 m

Use of (d,p) reactions for determination of O in WOx films

16O(d,p)17O0.85 MeV d mylar =12.8 mstandard 6.85·1017 O on Ta

p1

p0

p1

12C(d,p)13C C from the surface

sample WOx with 9.7·1016 O

CO/CW varying from 0.02 to 0.15, established correlation between pressure and O concentration

Planned PIGE applications

HPGe @ 135°20%, 2 keV @ 1.33 MeV

SB detector @ 165°

beam

FC

SB detector @ 45°

Si(Li) detector @ 150° forhigher energy x-rays 80 mm2, 155 eV @ 5.9 keV

SDD x-ray detector forlow energy X-rays20 mm2, 135 eV @ 5.9 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 isFor 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

10B

11B

19F Eγ=197 keV

23Na E=440 keV

24Mg

25Mg

27Al 27Al(p,p’γ)27Al (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