1. Text optional: Institutsname Prof. Dr. Hans Mustermann www.fzd.de Mitglied der Leibniz-Gemeinschaft Member of the Helmholtz Association High-Speed PIXE Fast Elemental Analysis with a Colour X-ray Camera Josef Buchriegler J.v. Borany, D. Hanf, S. Merchel, F. Munnik, S.H. Nowak, A.D. Renno, O. Scharf, R. Ziegenrücker ICNMTA, 11 th July 2014, Padova

2. 11 th July 2014, Padova 2 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association © Google Earth Dresden Padova Overview

3. 11 th July 2014, Padova 3 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Outline 1. Motivation Needs for a new PIXE set-up, Competitive methods 2. Experimental set-up IBC-overview, High-Speed PIXE set-up, SLcam ® 3. Data evaluation iXCC-Imager, GeoPIXE 4. First results Lateral resolution, Trace element detection 5. Summary & Outlook

4. 11 th July 2014, Padova 4 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Motivation Why new analysis methods should be developed?  urgent requirement for resource technology for exploration, mining, sustainable use and recycling of mineral and metalliferous resources due to:  rising energy costs  increasing environmental protection requirements  declining quality of geogenic resources  growing demand for metalliferous raw materials Source: Stephen Codrington

5. 11 th July 2014, Padova 5 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Motivation How new analysis methods should be developed? Foundation of Helmholtz Institute Freiberg for Resource Technology (in June 2011): joint venture between TU Bergakademie Freiberg & Helmholtz-Zentrum Dresden-Rossendorf aim of the new institute:  research of new technologies designed for: utilize resources more efficiently assure supply of raw materials environmentally friendly technologies

6. 11 th July 2014, Padova 6 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Motivation Why a new PIXE analysis method should be developed? Analytical chain for chemical analysis at Helmholtz Institute Freiberg: * under construction

7. 11 th July 2014, Padova 7 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Motivation How High-Speed PIXE can be competitive?  fast laterally resolved elemental information  high sensitivity for trace elements (concentrations < 0.1 at.%)  high throughput  large/heavy samples  grain size determination, intergrowth analysis, etc. High-Speed PIXE novel combination of PIXE as analytical method position sensitive detector  pixel-detector X-ray optics  polycapillaries fast data acquisition system established evaluation software  GeoPIXE

8. 11 th July 2014, Padova 8 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Experimental set-up Ion Beam Center overview Proton beam Scanning system Beam diagnostic chamber Sample chamber SLcam ® Data acquisition  approximately 90 m from ion source to sample surface  2 – 4 MeV protons  up to 1 µA current  un-scanned spot-size: 0.25 × 1.00 mm² Optical microscope Quadrupole

9. 11 th July 2014, Padova 9 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Experimental set-up High-Speed PIXE set-up A. Renno, D. Hanf, O. Scharf Proton beam Scanning system Beam diagnostic chamber Sample chamber SLcam ® Data acquisition Optical microscope Quadrupole 25 cm

10. 11 th July 2014, Padova 10 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Experimental set-up Classical µ-beam set-up Object 50x50 μm 2 Aperture 1x1 mm 2 Lens Sample surface High-energy proton beam (3 µA)  focused beam (1-5 µm) and scan across sample  big detector as close as possible to sample proton current on sample: 0.5 nA Sample surface High-energy proton beam (<1 µA)  broad beam  use of pixel detector (pnCCD)  local fields of view defined by suitable X-ray optics  combining X-ray optics and pnCCD:  laterally resolved PIXE images New approach: position sensitive detector & X-ray optics

11. 11 th July 2014, Padova 11 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Experimental set-up Functional principle sample surface tilted by 15°:  undistorted PIXE images  high X-ray yield two types of polycapillary optics: 1. straight capillaries  high depth of focus 2. conical capillaries  6:1 magnification Ø 19 mm

12. 11 th July 2014, Padova 12 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Experimental set-up SLcam ® NameValue number of pixel264 × 264 = 69 696 pixels size48 × 48 µm² image area12 × 12 mm² frame rate1000 Hz sensitive energy range2 – 20 keV active sensor thickness450 µm energy resolution152 keV @ Mn K α quantum efficiency >95% @ 3-10 keV >30% @ 20 keV window50 µm Be X-ray optics parallel (76 mm, 1:1) conical (82 mm, 6:1)

13. 11 th July 2014, Padova 13 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Data evaluation iXCC-Imager: real-time data analysis (IFG X-Ray Colour Camera) Geological sample “Kischa” (S04): 70 minutes @ ~300 nA  22×10 6 events

14. 11 th July 2014, Padova 14 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Data evaluation iXCC-Imager: real-time data analysis (IFG X-Ray Colour Camera) ~4 cm Ti K α Ca K β Cl K α K K α Mn K α Si K α 12 mm

15. 11 th July 2014, Padova 15 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Data evaluation Limits of iXCC-Imager: Overlapping peaks Intensity 10 6 10 5 10 4 10 3 0 4 8 12 16 20 keV Energy  Geological sample “Columbite” (S20): 4.5 hours @ ~300 nA  113×10 6 events 12 mm

16. 11 th July 2014, Padova 16 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Data evaluation GeoPIXE: Established evaluation software for geological samples Quantitative evaluation: detector properties sample properties (matrix) corrections for the optics X-ray line model background model pileup correction  Deconvolution of spectra 12 mm GeoPIXE iXCC

17. 11 th July 2014, Padova 17 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association First results Visual lateral resolution  Visual lateral resolution ~67 µm  intensity along green line Measurement of known structures: 67 µm Cu-stripes on Si-wafer spacing: 200 / 135 / 67 µm Px Cu-stripes (S08): 97 minutes @ ~500 nA  363×10 6 events pixel 3 mm

18. 11 th July 2014, Padova 18 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association “Cr on Si” (S16): 75 minutes @ ~400 nA  120×10 6 events  Sigmoid fits Calculated lateral resolution  intensity perpendicular to Cr-edge Cr-pattern on Si-wafer First results Line-Nr.Edge positionWidth (0.12-0.88) 6795.090.9 6895.211.3 6995.081.4 7095.001.5 7194.960.9 7294.931.5 7394.792.3 7494.791.4 7594.812.2 7694.922.2 7794.861.7 7894.711.6 Mean(94,93±0,15) px(1,58±0,47) px  Calculated lateral resolution: (76±23) µm pixel

19. 11 th July 2014, Padova 19 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association First results Cassiterite (Tin Stone) proton energy: 3 MeV current: ~ 700 nA meas. time: ~ 45 min Ta-Lα concentration map (<0.1 at.%) Trace element detection in geological samples

20. 11 th July 2014, Padova 20 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Summary & Outlook  Summary  new PIXE set-up built at HZDR  novel combination of SLcam ® and PIXE  motivation: resource technology  comparison with competitive methods  first assessment of lateral resolution  promising results with trace elements  Outlook o quantitative evaluation  accurate fluence monitoring o automation o windowless operation  lighter elements (Z<16) o full integration of GeoPIXE:  concentration maps in real-time

21. 11 th July 2014, Padova 21 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Acknowledgements This work is supported by Marie Curie Actions - Initial Training Networks (ITN) as an Integrating Activity Supporting Postgraduate Research with Internships in Industry and Training Excellence (SPRITE) under EC contract no. 317169 Helmholtz-Zentrum Dresden-Rossendorf, Dresden Shavkat Akhmadaliev Johannes von Borany Daniel Hanf Silke Merchel Frans Munnik Axel Renno René Ziegenrücker Operator team IFG Institute for Scientific Instruments, Berlin Stanisław H. Nowak Oliver Scharf Thank you for your attention !

22. 11 th July 2014, Padova 22 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Homogeneity Focused beam on Cu-plate 0.9 mm 1.7 mm

23. 11 th July 2014, Padova 23 Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | j.buchriegler@hzdr.de Member of the Helmholtz Association Homogeneity Broad beam on Cu-plate 12 mm