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The PIGE technique at ATOMKI and its applications in archaeometr y Árpád Zoltán Kiss
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The PIGE technique at ATOMKI and its applications in archaeometry
Árpád Zoltán Kiss Institute of Nuclear Research of the Hungarian Academy of Sciences
ATOMKI, Debrecen
IAEA 1st Research Coordination Meeting onReference Database of Cross Sections for PIGE Spectroscopy
IAEA Headquarters, Vienna, Austria, 16-20 May 2011
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OUTLINE
Introduction:
The Section of Ion Beam Physics, ATOMKI
From nuclear gamma-spectroscopy to PIGE in ATOMKI
Thick target gamma yields for PIGE
PIGE cross section measurements
Depth distribution measurements
Planned work in the frame of PIGE CRP
Examples of the application of PIGE in archaeometry
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SECTION OF ION BEAM PHYSICS
Nuclear Astrophysics GroupLaboratory of Ion Beam Applications
RESEARCH PERSONNELparticipating in the IAEA PIGE CRP
László CsedrekiGyörgy GyürkyGusztáv Áron SzikiZita SzikszaiImre Uzonyi
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The 5MV VdG accelerator
Beam: H+, D+, 4He+
Energy range: 0.6-3.8 MeV
Home made particle accelerators
from the 1970’s
The 1 MV VdG accelerator Beam: H+, 4He+ 12C+, 14N+
Energy range: 0.2-1.5 MeV
MGC-20 Cyclotron
SECTION OF ION BEAM PHYSICSInstrumentation
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ATOMKI Laboratory of Ion Beam Applications, Debrecen
macro-PIXE
Nuclear microprobe
PIGE/DIGE
DIGE or d-PIGE= deuteron induced gamma-ray emission
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Scanning Nuclear Microprobe (VdG-5 0o beamline)
Oxford Microbeams Ltd. 1.5 um x 1.5 um beam size HPT XZY-stage two-axis goniometer
PIXE, PIGE, RBS, STIM techniques Simultaneous u-PIXE and PIGE
measurements of heavy and light elements
Applications:: Geology Archaeology Materials science Characterisation of single aerosol
particles Micro-machining
(STIM = scanning transmission ion microscopy)
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Beamline for gamma spectroscopy (VDG-5 J30o)
Applications: Nuclear astrophysics p-PIGE, d-PIGE
Turntable for 2 Ge detectors 5 cm thick lead shielding
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Gamma and X-ray detectorsHPGe 40% (ORTEC), HPGe 20%(CANBERRA), Clover 120%, NaI(Tl)
X-ray detectorsSi(Li) and SUTW Si(Li)
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Leybold UINIVEX 350 vacuum coating system
Laboratory for sample preparation
Zeiss Axio Imager Optical Microscopewith CCD digital camera
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FROM GAMMA-SPECTROSCOPY to PIGE in ATOMKIExamples I.
Study of radiative gamma capture reactions (in collaboration with the University of Helsinki)
DSA measurement of short lifetimes in27Al. A., Bister M., Luukkainen A., Kiss Á. Z., Somorjai E.: Anttila Nucl.Phys. A 385 (1982)194.
The reaction 36S(,)40Ar: yield curve, excitation energies and decay of 40Ar resonance levels, Józsa M., Kiss Á.Z., Koltay E., Nyakó B. M. , Somorjai E., Keinonen J., Nucl. Phys. A 456 (1986)365.
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Cross section measurements in nuclear astrophysics(Collaboration with Bochum, LUNA, etc)
Absolute measurement of the 5/2+ resonance of 36Ar(p,)37K at Ep=918 keV. Mohr P., Oberhummer H., Gyürky Gy. , Somorjai E., Kiss Á. Z., Borbély-Kiss I., Phys. Rev. C 59 (1999)3:1790.
FROM GAMMA-SPECTROSCOPY to PIGE in ATOMKI Examples II.
Not for direct use in PIGEbut experience gained useful also for PIGE
Proton capture cross section of Sr isotopes and their importance for nucleosynthesisof proton-rich nuclidesGy. Gyürky, E. Somorjai, Zs. Fülöp, S. Harissopulos and P. Demetriou, T. Rauscher, Phys.Rev. C64 (2001) 065803
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Extension of the work done in Helsinki
Ep: 1.7, 2.4, 3.1, 3.8, 4.2 MeVElements: Li – Sc (except Ne, Ar)
Thick target gamma-yields for p-PIGE
THE PIGE TECHNIQUE AT ATOMKIearlier results
Results published in the form of spectra…
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… and in tabulated form.
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Thick target gamma-yields for d-PIGE(in collaboration with LRMF, Paris)
Deuteron energy interval: 0.7-3.4 MeV
Elements: Li – Sc (except Ne, Ar)
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G. A. Sziki, A. Simon, Z. Szikszai, Zs. Kertész, E. Dobos, Nucl. Instr.Meth. B 251 (2006) 343
Gamma ray production cross-sections for d-PIGE
Reactions and most dominant -lines
6Li(d,p)7Li, 478 keV (Li)9Be(d,n)10B, 718 keV (Be) 11B(d,p)12B, 953 keV (B)
1674 keV (B) 16O(d,p)17O 871 keV (O) 19F(d,p)20F 656 keV (F)
D e u te ro n e n e rg y [k e V ]
0 5 0 0 1 0 0 0 1 5 0 0 2 0 0 0
Cro
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ectio
n [m
barn
/sr]
0
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1 0
1 5
2 0
D e u te r o n e n e r g y [k e V ]
0 5 0 0 1 0 0 0 1 5 0 0 2 0 0 0
Cro
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ect
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[m
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r]
0
2 0
4 0
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1 6 0
D e u te ro n e n e rg y [k e V ]
0 5 0 0 1 0 0 0 1 5 0 0 2 0 0 0
Cro
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ectio
n [m
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/sr]
0
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1 0
1 5
2 0
2 5
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3 5D a ta fro m R e f. [1 4 ]T h is w o rk (m e a s u re d )C o n tro l m e a s u re m e n tsT h is w o rk (e x tra p o la te d )
D e u te ro n e n e rg y [k e V ]
0 5 0 0 1 0 0 0 1 5 0 0 2 0 0 0C
ross
sec
tion
[mba
rn/s
r]
0
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1 0
1 2
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D e u te r o n e n e r g y [ k e V ]
0 5 0 0 1 0 0 0 1 5 0 0 2 0 0 0
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[m
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0
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C o n t ro l m e a s u re m e n ts
C o n t ro l m e a s u re m e n ts
C o n t ro l m e a s u re m e n ts
C o n t ro l m e a s u re m e n ts
T a r g e t : L iF
T a r g e t : B e
T a r g e t : L iB O 2
T a r g e t : t i t a n iu m - o x id e
T a r g e t : L iF
E = 6 5 6 k e V
E = 8 7 1 k e VE = 9 5 3 k e V
E = 1 6 7 4 k e V
E = 4 7 8 k e V
E = 7 1 8 k e V
9 B e ( d ,n ) 1 0 B
1 6 O ( d ,p ) 1 7 O
6 L i( d ,p ) 7 L i
1 1 B ( d ,p ) 1 2 B
1 9 F ( d ,p ) 2 0 F
D e u te ro n e n e rg y [k e V ]
0 5 0 0 1 0 0 0 1 5 0 0 2 0 0 0
Cro
ss s
ectio
n [m
barn
/sr]
0
5
1 0
1 5
2 0
D e u te r o n e n e r g y [k e V ]
0 5 0 0 1 0 0 0 1 5 0 0 2 0 0 0
Cro
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ect
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[m
ba
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r]
0
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1 2 0
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1 6 0
D e u te ro n e n e rg y [k e V ]
0 5 0 0 1 0 0 0 1 5 0 0 2 0 0 0
Cro
ss s
ectio
n [m
barn
/sr]
0
5
1 0
1 5
2 0
2 5
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3 5D a ta fro m R e f. [1 4 ]T h is w o rk (m e a s u re d )C o n tro l m e a s u re m e n tsT h is w o rk (e x tra p o la te d )
D e u te ro n e n e rg y [k e V ]
0 5 0 0 1 0 0 0 1 5 0 0 2 0 0 0C
ross
sec
tion
[mba
rn/s
r]
0
2
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1 0
1 2
1 4
D e u te r o n e n e r g y [ k e V ]
0 5 0 0 1 0 0 0 1 5 0 0 2 0 0 0
Cro
ss s
ect
ion
[m
ba
rn/s
r]
0
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C o n t ro l m e a s u re m e n ts
C o n t ro l m e a s u re m e n ts
C o n t ro l m e a s u re m e n ts
C o n t ro l m e a s u re m e n ts
T a r g e t : L iF
T a r g e t : B e
T a r g e t : L iB O 2
T a r g e t : t i t a n iu m - o x id e
T a r g e t : L iF
E = 6 5 6 k e V
E = 8 7 1 k e VE = 9 5 3 k e V
E = 1 6 7 4 k e V
E = 4 7 8 k e V
E = 7 1 8 k e V
9 B e ( d ,n ) 1 0 B
1 6 O ( d ,p ) 1 7 O
6 L i( d ,p ) 7 L i
1 1 B ( d ,p ) 1 2 B
1 9 F ( d ,p ) 2 0 F
Thin samples: ~ 10-70 ug/cm2
Vacuum evaporation orDC reactive magnetron sputteringThin film RBS analysis
Standards:LiBO2, LiF, LiNO3, BN, NH4BF4, BeO, CaF2
Deuteron energy: 0.6-2 MeVEnergy steps: 20-50 keV
Estimated accuracy: 5-10%
depending on Ed
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Depth distribution of fluorine in implanted standard samples
Samples: fluorine implanted into silicon wafer
energy and dose: 2 keV, 11015 at.cm-2 100 keV, 11015 at.cm-2
Eres = 872 keV
Ibeam = 9 nA
Dbeamspot = 1 mm
Detector: 10 cm 10 cm NaI(Tl)Ddet-sample: 1cm=0
Experimental conditions:
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Overall view of the 19F(p,)16O excitation curve at =90°, normalized to a 3.8 g/cm2 F target, 60 C per point; 3”3” NaI(Tl) detector at 7 cm; detected E>4.7 MeV. [D. Dieumegard, B. Maurel, G Amsel, NIM 168 (1980) 93.
Overall view of the 19F(p,)16O excitation curve at =90°, normalized to a 3.8 g/cm2 F target, 60 C per point; 3”3” NaI(Tl) detector at 7 cm; detected E>4.7 MeV. [D. Dieumegard, B. Maurel, G Amsel, NIM 168 (1980) 93.
Excitation curve and used resonance
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Results:
Ion ranges of 3keV I in Si (SRIM calculation)
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PLANNED EXPERIMENTAL WORK in the frame of the
IAEA CRP Reference Database of Cross Sections for PIGE Spectroscopy
To obtain accurate experimental cross section data accurate determination needed:
- bombarding particle energy
- collected charge- number of bombarded target nuclei- efficiency of gamma detection
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Planned new target chamber on gamma spectroscopy beamline
Positions for sample and calibration target Accurate measurement of beam current Gamma detector – target distance
and detection angle to the beam direction
easily variable Possibility to measure RBS simultaneously
Target validation is possible in the nuclear microprobe: micro-PIXE/RBS
Cross section measurements
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Effect of various factors (experimental, matrix, etc.) influencing analytical accuracy of PIGE data.
Questions to be answered
What detector angle to the beam axis to be used?
In literature one can find: 0, 30, 45, 55, 60, 90 and 135 degrees
What is the detector solid angle?
What about d-PIGE cross section measurements?
Further possibility to investigate:
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Study of obsidian glasses
The aim of the work: to find sub-groups among the classified obsidian sources of the volcanic Tokaj Mountains (NE Hungary-E
Slovakia).
PIGE: 3.5 MeV proton energy, PIXE: 2.0 MeV
Improvenments in detection technique:Clover-BGO detector system
Application of PIGE in archaeometry(examples)
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Investigation of classical ring-stones and their imitations
In 17-18th c. Europe, a great interest towards the Greak and Roman art and culture. Great number of classicizing style objects or precise imitations .Nowodays in museums they are often mixed with the originals. Hard to make difference between them.
Primarily made from minerals or glass pastes.
In the later centuries different sorts of artificial masses also appeared as
base materials.
The determination of elemental compositions can make
differences betwen original artefacts and later produced
copies.
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PIXE/PIGE analysis similar to obsidians
Concentration correspondences for Na – Al (both normalized to Si)
Similarity dendogram for specimens using PIXE
data for elements occuring in each sample
One of the results:„Sacrificing Amor” is made of
glassy material.
Boron content indicates that the glass-pastecan not be a Roman origin.
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Investigation of incrusted pottery
• clay surface is incised to form a pattern,
• coloured (white) substance is pressed into the resulting lines,
• after burning: stable incrustation on the pottery
a very decorativetype of ornamentation
Questions to be answered: Can we identify the material used for this type of decoration? Can we observe regional/temporal differences in the composition of the material used for the decoration?
micro-PIXEC to Fe detected simultaneously by UTW and Be-W Si(Li)
micro-d-PIGE for N determination
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obtained in the frame of FP7 project CHARISMA
Incrusted pottery (Bükk culture)
Determination of fluorine contentIn the incrustationMicro-PIXE/PIGE simultaneously
Archaeological glass sealsproduced from ca. 1750-1850.(Finnish Glass Museum)All elements above C measured by PIXE
Monitoring the presence of boronPIXE/PIGE simultaneously
Recent results
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Thank you for your attention!