Development of single photon counting pixel detectors for synchrotron radiation applications

1. Development of single photon counting pixel detectors for synchrotron radiation applications Swiss Light Source / PSI SPring-8, Japan Hidenori Toyokawa Japan Synchrotron Radiation Research Institute / SPring-8 2.4 GeV storage ring First beam: August 2001 User operation: from October 2001 8 GeV storage ring First beam: March 1997 User operation: from October 1997 SPring-8 and the Switzerland's Paul Scherrer Institute (PSI) signed the MOU on May 1999 to promote advanced synchrotron radiation research.

2. PILATUS project • PILATUS (Pixel Apparatus for the SLS) is a challenging project to develop a large area single photon counting pixel detector for synchrotron radiation experiments by the PSI. • SLS detector group are sharing laboratories with CMS pixel group. • SPring-8 has been taking a part in the PILATUS project since 2001, based on the MOU. Pixel Apparatus for SPring-8 • Outline of my talk: • Features of pixel detectors • Applications at SPring-8 & SLS • Summary and outlook Mt. PILATUS

3. Existed 2D detectors for Synchrotron Radiation Applications • Position sensitive 2D detectors are powerful devices for use in synchrotron radiation experiments. Imaging plates are representative of them, and CCD-based detectors have become a major tool for protein crystallography recently. • These detectors, however, record X-ray intensity by integrating the energy deposited by X-ray photons. • Conventional Si, Ge, and NaI detectors are still essential instruments, when fluorescence background has to be rejected by energy discrimination, for example. • The readout time of CCD is in the second range, and that for imaging plate is minutes. It is often so inefficient and so time consuming.

4. 0.2 mm X-rays Pixel sensor 0.2 mm 0.3 mm Sensor Chip CMOS readout chip Bump Bonds Advantage for Pixel Detector • In this respect, the single photon counting pixel detector is regarded as a new generation of X-ray detectors. The most important features are the following. • No dark current, no readout noise and energy discrimination, resulting in maximum dynamic range. • High quantum efficiency. • Short readout time.

5. PILATUS 100 K Detector System(Single module) Complete X-ray Camera System,including Power- supply, PC, Software Radiation hard design No of pixels: 487 x 195 = 94’965 pixel Pixel size: 172 x 172 mm2 Dynamic Range/pixel: 20 bits Read out time: Tro = 2 ms @ 67 MHz Energy Range: 3 – 30 keV Lower discrimination Total Power Consumption: 15 W Frame Rate, PCI card Readout system: 200 Hz Air cooled, very simple operation Electronic shutter, external synchronization

6. PILATUS-II chip architecture • Radiation hard design • 60 × 97 = 5820 pixels • Pixel size 172 ×172 mm2 • Chip size 17.54 ×10.45mm2 • 20 bit counter/pixel (1,048,575 X-rays) • 6 bit DAC for threshold adjustment

7. PILATUS II Module 1 Hamamatsu Sensor 16 PILATUS II Chips (83.76 x 33.54 mm2) Hybrid from Dyconex Mechanical Support Module Control Board

8. The fundamental unit of the detector is the module, consisting of a single fully-depleted monolithic silicon sensor (Hamamatsu 6” wafer) with an 8 × 2 array of readout chips bump bonded to it. The sensor thickness is 320 mm. At 8 keV the absorption Si-sensor is nearly 100 % of the incoming radiation; at 12 keV 75 % of the radiation is stopped. CMOS is UMC 0.25 mm technology 8” wafer 380 or 720 mm in thickness. Bump-bonding was performed at the PSI. Bump bonding quality Total : 200 modules 0 defect : 5 0 - 0.01% : 67 0.01 - 0.1% : 46 (including sensor defect) Bump-Bonded Module with 16 chips

9. Analog performance

10. Comparator Calibration

11. Comparator Calibration

12. Threshold dispersion

13. Threshold dispersion

14. Rate performance

15. SPring-8 Bemline map

16. M. Yonemura, T. Osuki, Corporate Research and Development Laboratories, Sumitomo Metal Industries H. Terasaki, Y. Komizo, Joining and Welding Research Institute, Osaka University M. Sato, H. Toyokawa Japan Synchrotron Radiation Research Institute In situ characterization of directional solidification process during welding was carried out using the time resolved X-ray diffraction technique with high frame rate measurements up to 100 fps. The crystal growth during the rapid cooling was caught in detail and employed a systematic peak profile analysis in order to acquire the essential information for controlling the weld microstructure. . Two-dimensional Time-resolved X-ray Diffraction Study of Directional Solidification in Steels at BL46XU

17. Time resolved X-ray diffraction patterns during weld cycle ■Initial stage : δ200//NbC220  (100)δ// (100)NbC ■Final stage : Matrix: preferred orientation, NbC: random Halo pattern (Liquid Phase) γ200 γ111 (e)1420℃ (a)200℃ δ110 NbC200 NbC311 NbC220 NbC111 (b)500℃ (f)1370℃ γ111 γ220 Cooling Heating (c)1400℃ γ200 δ200 γ111 γ111 NbC220 δ110 (g)1150℃ (d)1660℃ NbC200 δ200 γ200 NbC111 δ110 (h)300℃ Halo pattern (Liquid Phase)

18. Ultra small angle X-ray scattering (BL19B2) Pilatus 5 min exposure Imagine plate 5 min exposure

19. X-ray diffractometer combining synchrotron radiation and pulsed magnetic fields up to 40 T at BL19LXU Y. Narumi,a K. Kindo,a K. Katsumata,b M. Kawauchi,c Ch. Broennimann,d U. Staub,d H. Toyokawa,e Y. Tanaka,b A. Kikkawa,b T. Yamamoto,c M. Hagiwara,c T. Ishikawa,b and H. Kitamura,b aISSP, University of Tokyo bRIKEN SPring-8 Center, Harima Institute cKYOKUGEN, Osaka University dSwiss Light Source, Paul Scherrer Institut eJapan Synchrotron Radiation Research Institute A synchrotron X-ray diffractometer incorporating a pulsed field magnet for high fields up to 40 T has been developed. The PILATUS-II SMD was used to store the diffracted X-rays. As a test of this instrument, X-ray diffraction by a powder sample of the antiferromagnet CoO is measured below the Neel temperature. A field-dependent lattice distortion of CoO due to magnetostriction is observed up to 38 T.

20. exposure exposure 10 ms 10 ms Experimental Setup: Powder Pattern at 20 T: X-ray diffraction at 40 Tesla @ Spring 8 Timing: magnetic pulse 5.5 ms (40T max) trigger 1 ms 1 s 1 s Magneto-striction of Cobalt-Oxide Delay 1.4 ms J. Narumi et al., J. Synchrotron Rad. 13 271-274 (2006)

21. Fluorescence XAFS (BL01B1) • Dynamic range • Dead time： 0.10 ms @ multi bunches mode • Count loss： 10 % @ 1*106 cps/pixel • Dynamic range： (1*106)*(8*104 pixel) ～ 1*1011 cps/ total area • Fluorescence XAFS spectra • Pt-L3 XAFS at BL01B1 • Sample: Pt foil • Measurement time: 120 sec • Future plan • Depth dependence XAFS： Grazing incident and position dependent fluorescence measurement

22. Reflection X-ray Incident X-ray Oil Scattered X-ray Water X-ray reflectivity of liquid-liquid interface (BL37XU) • Rapid measurement • Separation from strong scattered BG • Usual：　point detector scanning • PILATUS： 2D measurement • Measurement time： less than 1/10 • Reflectivity of liquid-liquid interface • Absorption => week signal • Scattering => background Reflection Scattering • Reflection profile • @ Qz = 0.4 (A-1) • Measurment time：　100 s • BL37XU @ 25 keV • Reflectivity of Hexane/Water interface

23. X-ray Detector Spot size: - Beam size and divergence - Mosaicity of the crystal - Distance sample-detector - Point spread function of detector 2q Diffraction pattern Diffracted beam Crystal rotation - 30-180 degree for complete data set - Currently: Discrete rotation, integration over certain rotation angle - Fine f-slicing with continuos sample rotation Resolution: × q = l Thaumatin (PDB code: 1LXZ) M.W. 22188Da Residues 207a.a. 2 2 d d sin( sin( ) ) Crystallized o Protein For d=l=1A 2q=60o Beam Beam Diffraction data Energy: 5-17.5 keV - reflect crystal symmetry group Intensity: >1012/s - orientation of the crystal-> orientation matrix 4 Focal spot size: Adjustable to - High dynamic range: >104 between strong and weak reflections mm2 >75 x 30 - Intensities need to be determined accurately (1%) Divergency: <375 x 70 µrad2 - Determination of amplitudes and phases leads (FWHM) to electron density maps Pixel Detectors for Protein Crystallography A major purpose of developing a large area pixel detector is for macromolecular crystallography. The PILATUS-6M) has 2463  2527 pixels covering 424 mm  435 mm with 5  12 modules.

24. PILATUS 6M Parameters • 60 modules fully functional • 3 billion transistors • Module alignement: < 1 pixel • Clock frequency 25 MHz (50 MHz final) • Readout time: 6ms, (2.54 ms final) • Image size 25 MB (32 bit) • Frame rate 4 Hz continuous -> > 100 MB/s on disk sustained (DAQ E. Eikenberry) • Shutter synchronization via external trigger input • Exposure timing defined by PILATUS detector • Online corrections

25. Ferritin Protein Crystal

26. Insulin Protein Crystal

27. Decagonal AlIrOs Quasicrystal

28. Samson Phase

29. Summary and outlook • We have been developing the large area single photon counting pixel detectors. • PILATUS-II 100K realizes a desired performance with a fast frame rate up to 200 Hz. It has wide application ranges, and several systems are already distributed to other synchrotron radiation facilities. • PILATUS-6M detector with the 5  12 modules for protein crystallography has been completed at SLS. • PILATUS-2M detector with the 3  8 modules for small angle scattering and other applications is under development. • PILATUS-XFS project starts this yser. • 75 mm × 75 mm pixel, > 10,000 fps

30. I would like to thank A. Bergamaschi, Ch. Broennimann, R. Dinapoli, E.F. Eikenberry, B. Henrich, M. Kobas, P. Kraft, M. Naef, H. Rickert, P. Salficky, B. Schmitt PSI, SLS Detector Group, Villigen-PSI, Switzerland R. Horisberger, et al… PSI, CMS-Pixel, Villigen-PSI, Switzerland M. Sato, M. Suzuki , H.Tanida T. Uruga, et al... JASRI, SPring-8, Japan Jared Winton, Bryn Sobott The University of Melbourne, Australia H. Niko University of Tokyo, SPring-8, Japan