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The PIGE technique at ATOMKI and its applications in archaeometr y Árpád Zoltán Kiss

The PIGE technique at ATOMKI and its applications in archaeometr y Árpád Zoltán Kiss Institute of Nuclear Research of the Hungarian Academy of Sciences ATOMKI , Debrecen. IAEA 1st Research Coordination Meeting on Reference Database of Cross Sections for PIGE Spectroscopy

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The PIGE technique at ATOMKI and its applications in archaeometr y Árpád Zoltán Kiss

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  1. 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 IAEA1st Research Coordination Meeting on Reference Database of Cross Sections for PIGE Spectroscopy IAEA Headquarters, Vienna, Austria, 16-20 May 2011

  2. 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

  3. SECTION OF ION BEAM PHYSICS Nuclear Astrophysics Group Laboratory of Ion Beam Applications RESEARCH PERSONNEL participating in the IAEA PIGE CRP László Csedreki György Gyürky Gusztáv Áron Sziki Zita Szikszai Imre Uzonyi

  4. SECTION OF ION BEAM PHYSICS Instrumentation The 5MV VdGaccelerator • 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

  5. ATOMKI Laboratory of Ion Beam Applications, Debrecen Nuclearmicroprobe PIGE/DIGE macro-PIXE DIGE or d-PIGE= deuteron induced gamma-ray emission

  6. Scanning Nuclear Microprobe(VdG-5 0obeamline) • 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 (STIM = scanning transmission ion microscopy) • Applications: • Geology • Archaeology • Materials science • Characterisation of single aerosol particles • Micro-machining

  7. Beamline for gamma spectroscopy(VDG-5 J30o) Turntable for 2 Ge detectors 5 cm thick lead shielding • Applications: • Nuclear astrophysics • p-PIGE, d-PIGE

  8. Gamma and X-ray detectors HPGe 40% (ORTEC), HPGe 20%(CANBERRA), Clover 120%, NaI(Tl) X-ray detectors Si(Li) and SUTW Si(Li)

  9. Laboratory for sample preparation Leybold UINIVEX 350 vacuum coating system Zeiss Axio Imager Optical Microscope with CCD digital camera

  10. FROM GAMMA-SPECTROSCOPYto PIGE in ATOMKI Examples 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.

  11. FROM GAMMA-SPECTROSCOPYto PIGE in ATOMKI Examples II. Cross section measurements in nuclear astrophysics (Collaboration with Bochum, LUNA, etc) Proton capture cross section of Sr isotopes and their importance for nucleosynthesis of proton-rich nuclides Gy. Gyürky, E. Somorjai, Zs. Fülöp, S. Harissopulos and P. Demetriou, T. Rauscher, Phys.Rev. C64 (2001) 065803 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. Not for direct use in PIGE but experience gained useful also for PIGE

  12. THE PIGE TECHNIQUE AT ATOMKI earlier results Thick target gamma-yields for p-PIGE Extension of the work done in Helsinki Ep: 1.7, 2.4, 3.1, 3.8, 4.2 MeV Elements: Li – Sc (except Ne, Ar) Results published in the form of spectra…

  13. … and in tabulated form.

  14. 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)

  15. Gamma ray production cross-sections for d-PIGE Thin samples: ~ 10-70 ug/cm2 Vacuum evaporation or DC reactive magnetronsputtering Thin film RBS analysis Standards:LiBO2, LiF, LiNO3, BN, NH4BF4, BeO, CaF2 Deuteron energy: 0.6-2 MeV Energy steps: 20-50 keV 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) Estimated accuracy: 5-10% depending on Ed G. A. Sziki, A. Simon, Z. Szikszai, Zs. Kertész, E. Dobos, Nucl. Instr.Meth. B 251 (2006) 343

  16. Depth distribution of fluorine in implanted standard samples Samples: fluorine implanted into silicon wafer energy and dose: 2 keV,11015 at.cm-2 100 keV,11015 at.cm-2 Experimental conditions: Eres=872 keV Ibeam=9 nA Dbeamspot= 1 mm Detector: 10 cm  10 cm NaI(Tl) Ddet-sample:  1cm =0

  17. Excitation curve and used resonance

  18. Results: Ion ranges of 3keV I in Si (SRIM calculation)

  19. 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

  20. 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

  21. 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: Effect of various factors (experimental, matrix, etc.) influencing analytical accuracy of PIGE data.

  22. Application of PIGE in archaeometry (examples) Study of obsidian glasses PIGE: 3.5 MeV proton energy, PIXE: 2.0 MeV Improvenments in detection technique: Clover-BGO detector system The aim of the work:to find sub-groups among the classified obsidian sources of the volcanic Tokaj Mountains (NE Hungary-E Slovakia).

  23. 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.

  24. 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-paste can not be a Roman origin.

  25. 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 decorative • type 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-PIXE C to Fe detected simultaneously by UTW and Be-W Si(Li) micro-d-PIGEfor N determination

  26. Recent results obtained in the frame of FP7 project CHARISMA Archaeological glass seals produced from ca. 1750-1850. (Finnish Glass Museum) All elements above C measured by PIXE Monitoring the presence of boron PIXE/PIGE simultaneously Incrusted pottery (Bükk culture) Determination of fluorine content In the incrustation Micro-PIXE/PIGE simultaneously

  27. Thank you for your attention!

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