Utilization of the RBI Tandem Accelerator Facility for Analytical Applications

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Utilization of the RBI Tandem Accelerator Facility for Analytical Applications Stjepko Fazinić Laboratory for Ion Beam Interactions Rudjer Bošković Institute, Zagreb, Croatia International Topical Meeting on Nuclear Research Applications and Utilization of Accelerators, Vienna, 4-8 May 2009 Satellite meeting II: Particle Accelerators in Analytical and Educational Applications Ruđer Bošković Institute, Zagreb, Croatia

Laboratory for Ion Beam Interactions, Rudjer Boskovic Institute, Zagreb, Croatia: I. Bogdanovic Radovic, M. Bogovac, I. Bozicevic, S. Fazinic, A. Gajski, M. Jaksic (head), M. Karlusic, Z. Pastuovic, Z. Perisa, Z. Siketic, N. Skukan, D. Spanja, T.Tadic, I. Zamboni Micanovic Faculty of Engineering, University of Rijeka: L. Mandic Department for Conservation and Restoration, Academy of Fine Arts: V. Desnica Croatian Conservation Institute, National Science Laboratory M. Braun, D. Mudronja Ruđer Bošković Institute, Zagreb, Croatia

History accelerators of the R. Boškovi ković Institute 1956 1973 1987 1956-200 kev neutron generator 1973-350 kev neutron generator (Still in use) 1962 1987 6 MV EN Tandem 2005-1 MV Tandetron 2005 1962 1987. Cyclotron (20 MeV deuterons) 2009-18 MeV proton cyclotron (PET isotopes)

Tandem accelerators facility PIXE/RBS

RBI Laboratory for Ion Beam Interactions Interactions of accelerated ion beams with materials Fundamental processes - Stopping of ions in solids and related effects - Inner shell ionization and X-ray emission processes - Ion scattering - Nuclear reactions Developments - data acquisition and control software and hardware (SPECTOR) - accelerator computer control (including remote operation) - design and constructions of end-stations Applications - Material characterisation (analysis) by IBA - Material modifications Ruđer Bošković Institute, Zagreb, Croatia

Ion Beam Analysis (IBA) NRA Nuclear reaction products Charge pulse IBIC PIGE γ rays Recoil nuclei ERDA Ion beam Transmitted particles STIM PIXE X-rays Forward scattered particles RBS SEI Backscattered particles Secondary electrons Light IL TARGET Concentrations and/or depth profiles: Elements - x-rays (PIXE) - backscattered particles (RBS) - recoiled ions (ERDA) Isotopes - gamma-rays (PIGE) - nuclear reactions (NRA) Density variations transmitted ions (STIM) Charge transport ion beam induced current (IBIC) Chemical bonds light (IL), x-rays (high resolution) Crystal structure channeling RBS, STIM, PIXE Morphology secondary electrons (SEI) Ruđer Bošković Institute, Zagreb, Croatia

Ion (nuclear) microprobe PIXE, RBS, ERDA, IBIC, STIM Coincidence scattering Ion hit detection (SE & IL) Focusing system quintuplet ME/q2 < 25 Equal demagnification 0.5 µm smallest beam size Ruđer Bošković Institute, Zagreb, Croatia

microprobe - inside the vacuum chamber

Microprobe ion beam object slits quadrupole focusing lens system sample Y scan generator X x-ray detector amplifier Y X X-ray energy spectrum Fe Ca S Pb elemental maps Ruđer Bošković Institute, Zagreb, Croatia

Example: Analysis of metal threads of a 17th century church textile with PIXE at the microprobe The left lamina contains more copper, whereas the two right ones are silver laminas. Ruđer Bošković Institute, Zagreb, Croatia

Example: Analysis of stone samples at the microprobe Conservation of St. Marko church portal total PIXE yield 900 800 700 600 500 400 300 200 100 total yield 0 1400 1200 1000 800 600 Ba Fe S -4000-3000 -2000-1000 0 depth (micron) Portal sample P1 Ba depth distribution (S1) Florentine method of cleaning and consolidation by soaking the stone in ammonium carbonate and barium hydroxide was used. Barium and sulfur concentration level variations with depth have been determined in samples taken from the portal after the treatment. 400 200 0-4000 -3500-3000 -2500-2000 -1500-1000 -500 0 500 1000 depth (micron) Sandstone sample treated in laboratory In addition, Ba depth profiles in sandstone treated by three different ways were measured. Ruđer Bošković Institute, Zagreb, Croatia

Analysis of pigment layers at the microprobe 2D element distribution of the pigment cross section sample taken from the red area of the painting. The light red layer exhibits high Hg and S concentrations (HgS cinnabar), while the dark red layer beneath shows presence of Pb, Al, Ca, but without Hg (either minium, or carmine).

Examples: Analysis of pigment layers at the microprobe Microsamples are the same as ones needed for optical mictroscopy techniques. Method is non-destructive and samples may be re-used. We analyse between 50 to 100 such samples per year. Ruđer Bošković Institute, Zagreb, Croatia

Example 2: STIM tomography module (1) Sample positioning on the axis of stepper motor using microscope (3) Measurement (2) Loading into the chamber (4) Reconstruction and visualization

Object rendering using AMIRA software

Single ions tool for charge injection and probe for micro - imaging of charge transport properties Frontal IBIC Scan area Bias voltage - + + - - + + - + - - + + + - - 16 O 12 C 7 Li alphas (Junction) Lateral IBIC Scan area (n) IBIC pulse (p) Grain boundaries Charge traps 1. Imaging of electronically active defects in Si, CVD diamond, CdTe, GaAs,... protons 2. Creation /structuring of defects change of charge transport properties: the example of Si pin diodes

PIXE/RBS scattering chamber PIXE, RBS, PIGE detectors simultaneous measurements SPECTOR data acquisition + computer controled sample changer PIXE RBS Beam shape is defined by the collimators (beam defining slits) and is usually from 1 to 8 mm Faraday cup PIGE Ruđer Bošković Institute, Zagreb, Croatia

Example: Analysis of samples taken from the surface of the stone material of the Roman remains in Split Samples analysed in vacuum at the IBA end-station Ruđer Bošković Institute, Zagreb, Croatia

Time of flight ERDA spectrometer x,y,z,θ θ manipulator T2 M2 TOF = T 1 T 2 = l 2 KE0 4M 1M 2 cos 2 φ K= 2 ( M1 + M 2 ) o o o o o L=523.4 mm T1 Vacuum chamber 2 Si E detector ERDA (Elastic Recoil Detection Analysis) TOF (time of flight) system for separation of scattered from recoiled ions (v,e) Depth resolution down to 5 nm Ion beams Cl, I (energies 10-50 MeV) Resolution of isotopes up to M = 28 11B 10B 7Li 1H 19F 16O 4He

TOF-ERDA Spectrum example Coincidence spectrum (E and TOF coincidence) obtained by bombarding Si/20Å Ta/100 Å AlNO/20Å Au Round robin sample by 35 MeV 35 Cl Sample tilt angle θ in = 17.5 35 Cl scattered from Si 56 Fe 35 Cl scattered from Fe 28 Si 14 N 12 C 16 O 27 Al 35 Cl scattered from Ta 35 Cl scattered from Au

High Resolution PIXE Simple high resolution wavelength dispersive crystal spectrometer with position sensitive proportional counter. Data acquisition by SPECTOR. vacuum chamber flat crystal PSPC detector He baloon

Example: High Resolution PIXE measured spectra of selected Ti and V compounds to investigate chemical effects on Kβ X-ray spectra

PIXE analysis in air For large/bulky objects and samples that cannot be exposed to vacuum Ruđer Bošković Institute, Zagreb, Croatia

Examples: Analysis of alloys Analysis in air Ruđer Bošković Institute, Zagreb, Croatia

Example: Analysis of pigments at the in-air end-station Fiorentino / white Fiorentino / blue C(%) AlK 1.66 SiK 1.05 P K 0.31 S K 0.03 ClK 3.20 K K 0.91 CaK 2.34 TiK 0.00 FeK 1.22 CuK 0.06 BaLA 0.00 PbLA 78.66 C(%) AlK 1.31 SiK 1.29 P K 0.36 S K 2.67 ClK 0.75 K K 0.35 CaK 1.17 TiK 0.08 FeK 1.05 CuK 50.09 BaLA 5.48 PbLA 18.81

New dual beam chamber Beam from Tandetron Beam from EN Tandem (still under construction) simultaneous modification + analysis Load lock xyz stage

SPECTOR home made Data acquisition /target positioning & beam scanning software

Computer control ACCEL6 for EN Tandem Van de Graaff and ACCEL1 for Tandetron accelerator - 16 bit AD/DA modules (controls for ion sources, accelerator and beam optics system) - 8 digital inputs, 8 digital outputs - Controls are based on TESTPOINT Capabilities: - Remote control (from remote computers) - Reads beam optics parameters from previous experiments - Calculates changes of parameters for change of energy and/or ion - Security interlock system

Remote experiments on accelerator Performance of experiments by expert users Access to accelerator control console Sample positioning and beam scanning Data acquisition Education and training for users unfamiliar with technique Viewer to accelerator control console Beam controls on/off Access to sample changer and data acquisition with limited access On-line tutorial Examples - IAEA trainees (in collaboration with the IAEA Seibersdorf Laboratory) - Laboratories starting PIXE - Remote Universities without experimental facilities Ruđer Bošković Institute, Zagreb, Croatia

Thank you