PSI with the Swiss Light Source SLS. Christian Broennimann. Paul Scherrer Institut 5232 Villigen PSI

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Solid State Detector Development at the Swiss Light Source Christian Brönnimann Group Leader SLS Detector Group Paul Scherrer Institut CH-5232 Villigen-PSI, Switzerland PSI with the Swiss Light Source SLS

Solid State Detector Development at the Swiss Light Source Goal: Show that solid state single photon counting detectors are excellent devices 1) Introduction 2) Mythen Detector for Powder diffraction 3) Pilatus Project Surface diffraction / SAX Protein crystallography Pilatus 6M 4) Ideas for the future

The Swiss Light Source Detector projects: X04SA: MS Beamline, PD Station, E=8-30keV: MYTHEN detector, large microstrip detector: X06SA: PX I Beamline, E=5-20keV PILATUS detector, large area pixel detector X04SA: MS Beamline, SD Station, E=8-30keV: Single PILATUS Module Energy range very well suited for Si-Detectors

Solid State Pixel and Microstrip Detectors Sensor: Si pn-junction p+ n+ n++ Al 3.6 ev to create 1 eh-pair 0.3mm, Pixel Detector (2D) 0.2 mm X-rays E drift Pixel Sensor - + V bia X-rays Readout Chips: Single Photon Counting Electronics s Bump Pad Cal Treshold correction CS Amp 1.7fF Global Tresh Microstrip Detector (1D) Microstrip Sensor - Comp + Enable/ Disable Analog Block Microstrip chip Ext/Comp Clock Ext Clock Hybrid Φ12 Clock Gen 15 bit SR counter Reset Digital Block RBI RBO 0.3 mm 0.2 mm Pixel Read-out Chip Sensor Chip Bump Bonds Signals Bond Pads Wire Bonds

Single photon counting hybrid pixel/strip detectors Properties: Energy range 4 30 kev No dark current No readout noise Excellent point spread function Short readout times: ms Suppression of fluorescent background Very good signal/noise ratio 100 90 80 70 n+=1um n+=2um Silicon Absorption n+=0.5 um Applications: Protein Crystallography Powder Diffraction Surface Diffraction Small Angle Scattering Challenges: Quality Stability Calibrations, i.e. the precision of the data 60 n+=5um 50 40 30 20 2.00 7.00 12.00 17.00 X-ray Energy [kev] Silicon is the optimal choice for SLS-Detectors

The Mythen Detector System (B. Schmitt) conventional analyser sample Angular coverage: 60 o No of channels: 15000 Angular resolution : 0.004 o Read-out time: 250 µs beam time resolved powder diffraction microstrip detector

The Mythen Detector System

In-situ peak profile analysis at SLS Beam Microstrip-detector In-Situ X-ray diffraction measurements of deformation mechanisms Intensity 7000 6000 5000 4000 3000 2000 1000 39.3 39.4 39.5 39.6 39.7 2θ

ED-Ni (26 nm by XRD) True Stress (GPa) 2.5 2.0 1.5 1.0 0.5 0.0 0 1 2 3 4 5 6 7 8 9 10 True Strain (%) Peak Position 40.68 40.66 40.64 40.62 40.60 40.58 40.56 0 1 2 3 4 5 6 7 8 9 10 True Strain (%) (222) FWHM 0.42 0.40 0.38 0.36 0.34 0.32 0.30 (222) 0.28 0 1 2 3 4 5 6 7 8 9 10 True Strain (%) In nanocrystalline Ni the peak broadening is entirely reversible upon unloading, deformation mechanism does not built up a residual dislocation network! as was predicted by large atomistic simulations H. Van Swygenhoven, Derlet, Budrovic, Van Petegem, Schmitt NUM/ASQ/SLS Science, 304 (2004) Nat. Mat., June (2004)

Mythen V2 (B. Schmitt) New 0.25 µm readout chip designed Features: 128 channels Low noise <240 ENC 6 bits for threshold fine-tuning High count rate: linear to >1MHz (measured with X-rays) 24 bit counter with variable length readout, readout time from 32 µs (4bit) to 64 µs (24bit) for entire chip/detector Frame rates of 10kHz are planned Current detector will be replaced by V2 Summer this year

The PILATUS Project PILATUS Module Typ I (Aug 2001) Module Data Active Area: 79.6 x 35.3 mm 2 (continuously sensitive) 157 x 366 = 57462 pixels 16 chips (radiation hard) Pixel size 0.217x0.217 mm 2 Readout-time: 6.7 ms Energy Range: Eγ >4.5 kev Minimum Threshold: 3 kev Threshold adjust per pixel Rate: ~10 khz/pixel 15-bit counter/pixel single photon counting, no readout noise

The Surface Diffraction Station at X04SA Point Detector Single Module Pixel Detector Frame rate 30 Hz Specimen Beam 6 Circle Diffractometer

Crystal truncation rods (CTRs) at X04SA surface-sensitive structural information Classic: Time-consuming scans with a point detector at points along the CTR New: About 50 times faster with the pixel detector

CTRs of the surface of SrTiO 3 27 CTRs with 1800 data points recorded in a few hours C. Schlepuetz et al, Improved data acquisition in grazing-incidence x-ray scattering experiments using a pixel detector, submitted to NIM A, Jan 2005

SAX Pattern of a polystyrene latex solution (H. Toyokawa, M. Suzuki SPring 8) Single X-ray Resolution!

PILATUS Module Typ II (readout electronics bended) Sensor Wire bonds Read-out chips Base plate Module Control Board MCB Al support Cable Flexprint 6/2 from Dyconex Modules can be overlapped 80 x 35 mm 2 continuous sensitive area 2 x 8 readout chips Power consumption: 7V/1.5 A -> 10.5 W Fabrication of 21 Modules: Mai 03- Sept 03

The PILATUS 1M Detector Largest pixel detector array for SR 6 banks a 3 modules, 1120 x 967 pixels Area: 21 x 24 cm 2 288 chips->~300x10 6 transistors Readout time: 6.7ms Currently 2 frames/s 2 frames/ s Active area: 85% Moderate count rates (<10kHz/pixel)

PILATUS 1M Detector at X06SA

Thaumatin crystal Data Taking: Data set: 120 o Exp Time: 4s Integration: 1 o Beam energy: 11.9 kev Beam intensity: 13.5% D Sample-Det: 128 mm Resolution: 1.4 Å Analysis: 3 data sets merged full geometrical correction Processed with XDS R obs : 8.9% (overall) Completeness: 90% (98% up to 1.6 Å)

Zoom in

SLS Detector Group Thaumatin electron density map Processing with XDS Refinement with SHELXL Completeness: 90.3% R sym 8.4% Resolution: 1.4 Å Refinement: R-Factor 28% blue contours: 2*Fo-Fc (2sigma) red contours: Fo-Fc (2sigma)

Fine φ-slicing with the PILATUS-Detector Conventional Integration Int φ Rocking curve Integrated intensity short readout-time φ Fine φ-slicing φ Continuous rotation -> no shutter no read-out noise Int Angular speed ω, Exposure time t φ=t*ω 0 Φ

Fine-phi slicing with continuous sample rotation (raw data)

Fine-φ sliced data-sets Thaumatin crystal, 11.9keV, continuous sample rotation 1s exposure, 6.2ms read-out time, 180 deg 50 images/deg (0.02 o /s) Complete data set ~ 9000s, 9000 frames data-set overexposed FWHM=0.12 o

PILATUS II Chip UMC_25_MMC process; Radiation hard design 150 x 150 µm2 60 x 97 pixels = 5820 pixels Pixel size 172 x 172 um2 17.540 x 10.450 mm2 Count rate: 1MHz/pixel 20 bit counter Counting timer circuit 6 bit DAC for threshold adjustment XY-adressable Analog output 100 MHz LVDS readout (Tro = 1.2 ms) Submitted 29.09.04 Received 1.12.04 4*106 Transistors

PILATUS II Pictures 150 x 150 µm 2

PILATUS II: Analog Frontend Amplifier Injected Signal: ~ 15.4 kev ~ 11.8 kev ~ 7.2 kev ~ 3.6 kev Settings: Aout of Pixel 0,0 (bottom left) Va+ = 1.2 V, (I pix = 13 µa) V rf = -0.2 V V rfs = 0.8 V < 300 ns

PILATUS II: Analog output of each pixel E cal = 12 kev Threshold scans of SLS08-Chip (w.o. Sensor)

Comparison PILATUS I PILATUS II Chip Calibrate Readback PILATUS I (3432 pixels, 5% defects) Calibrate Readback PILATUS II ( Vcal= 0.5V, 5820 pixels, 0 defects) Calibrate Readback PILATUS II ( Vcal = 0.4 V)

The PILATUS 6M No of Modules 60 Module size 487 x 195 pixels (90k) Detector Size 431 x 448 mm 2 No of Pixels 2527 x 2463 pixels (6M) Spatial resolution 0.172 x 0.172 mm 2 Dynamic range: 20bits Readout time ~2ms Frame rate 5-10 Hz Rate 1 MHz/pixel Spatial distortion Flat geometry Dead area ~8.4 % (7 pixels in x, 17 pixels y) Status: Currently under design

SLS Detector Group PILATUS 6M No of Modules 60 Module size 487 x 195 pixels (90k) Detector Size 431 x 448 mm 2 No of Pixels 2527 x 2463 pixels (6M) Spatial resolution 0.172 x 0.172 mm 2 Dynamic range: 20bits Readout time ~2ms Frame rate 5-10 Hz Rate 1 MHz/pixel Spatial distortion Flat geometry Dead area ~8.4 % (7 pixels in x, 17 pixels y) Status: Currently under design

X-rays on detector: Ideas for the future Frame based: t Expose 1 RO1 Transfer 1Exp 2 RO2 Transfer 2Exp 3 Pilatus II Module: 100k pixel --> 200kBytes / frame Frame rate dependent on transfer time With fast PCI-DAQ cards: 100MBytes/s No of Modules Frame Rate 2 Modules -> 125 Hz 10 Modules (1M Pixels) -> 30 Hz 60 Modules (6M) -> 5 Hz

Region of Interest Readout (ROI) Implemented on chip level RO: 10x10 pixels -> 20 us Transfer: -> 100 us Exposure = 100 us -> 100 X-rays/peak, BG=? 100 10x10 Chip Frame rate -> 8000 Hz Frame based, gated operation 50 Laser pulse SLS, Hybrid mode 100ns 1 us RO1 Possible with Pilatus 6M Modules

Higher frame rates -> data reduction! Image compression: e.g. difference btw neighbouring pixels in image, read out only necessary bits Usual compression algorithms -> data reduction by a factor of 2.5 For short exposures, suppress zeros maybe factor of 10 Problem: BG extremely sample and position dependent New Science with New Detectors, ESRF, Grenoble, 9./10. 2. 2005 34

Fast framing pixel detector for the coherent SAXS BL Good quantum efficiency from 3 15 kev Rad-hard readout chip Single photon counting Pixel size: 40 x 40 to 60 x 60 µm 2 Count rate: 1 MHz/pixel -> 3 x 10 8 x-rays/mm 2 /s Array size: > 1000 x 1000 Pixels Frame rates: 100 Hz for full readout >1 khz, with data compression read-out Currently under evaluation New Science with New Detectors, ESRF, Grenoble, 9./10. 2. 2005 35

Conclusion Single Photon Counting Solid state detectors are still under development enable new experiments deliver excellent data can be developed application specific

Acknowledgements R. Dinapoli, E.F. Eikenberry, B. Henrich, G. Hülsen, P. Kraft, M. Naef, H. Rickert and B. Schmitt, PSI, SLS Detector Group, Villigen-PSI, Switzerland H. Toyokawa, M. Suzuki JASRI, Spring 8, Japan B. Patterson, C. Schulze-Briese, T. Tomizaki, C. Pradervand, A. Wagner, P. Willmott PSI, Villigen-PSI, Switzerland R. Horisberger, S. Streuli, F. Glaus PSI, Villigen-PSI, Switzerland