A single photon counting pixel detector system for synchrotron - - PowerPoint PPT Presentation

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

A single photon counting pixel detector system for synchrotron radiation applications

• H. Toyokawa

Japan Synchrotron Radiation Research Institute / SPring-8

SPring-8, Japan Swiss Light Source / PSI SPring-8 and the Switzerland's Paul Scherrer Institute (PSI) signed the MOU on May 1999 to promote advanced synchrotron radiation research. 8 GeV storage ring First beam: March 1997 User operation: from October 1997 2.4 GeV storage ring First beam: August 2001 User operation: from October 2001

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

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.

• SPring-8 has been taking a part in the

PILATUS project since 2001, based on the MOU.

• Outline of my talk:

– Futures of existed detectors and pixel detectors – PILATUS-I with DIMILL technology – PILATUS-II with 0.25 µm technology – Summary and outlook

• Mt. PILATUS

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

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.

• 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.

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

Advantage for Pixel Detector

ADC

Q V V Threshold

X-rays

• n detector

Integrating detector

t E

Single photon counting detector

Amplifier

• utput

Comparator

• utput

Counter

• 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.

Pixel sensor X-rays

CMOS readout chip

0.2 mm 0.2 mm 0.3 mm

Bump Bonds Sensor Chip

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

PILATUS-I

• The developed pixel detector consists of a

number of detector modules.

• The 1st module (PILATUS-I SMD) has been

developed in August 2001, and the 1M pixels large area detector with 3 × 6 modules in November 2003.

• Although the PILATUS-I detector was a

prototype with about 5% defective pixels in the readout chip (PILATUS-I chip) due to the DMILL technology, it realized a sufficiently high performance to allow the methodological study of its fields of applications.

• We could study how to integrate the

detector, how to operate in synchrotron radiation applications and how to analyze the data.

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

Single Module Detector with Pilatus I Chip

single module 366 x 157 pixels Area: 81 x 36.6 mm2 16 chips Readout time: 6.7ms @ 10 MHz up to 30 frames/sec

• An array of 2 × 8 custom CMOS readout chips is indium bump-

bonded to the sensor.

• Each pixel contains a charge-sensitive amplifier, a single level

discriminator and a counter. An individual pixel is thus capable of being operated in a single photon counting mode.

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

Two-dimensional Time-resolved X-ray Diffraction Study of Directional Solidification in Steels at BL46XU

• 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 the PILATUS-I SMD. 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. Then, high frame rate measurements up to 100 fps were performed with the PILATUS-II

• SMD. Data is under analysis.

Water-cooled copper plate Arc discharge Torch scan（ ～1mm/s) X-ray beams（ 18KeV） Power:10V, 150A θ=20° Cooling water To cooling tower Specimen（ 12mmt） 2θ=35° Silicon pixel detector Silicon pixel detector

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

Time Time-

• resolved diffraction pattern of the Fe

resolved diffraction pattern of the Fe-

• 0.05C alloy

0.05C alloy

γ220 γ220 α211 γ311 α200 α211 α220 (b) ～1450℃ (c) ～600℃ α200 γ220 α211 α220 γ311 (d) ～500℃ (e) ～400℃ δ220→

A single-phase γ-Fe region first appears at about 1450℃. Then the diffraction pattern shifts to a higher angle suggesting an improvement of

• crystallinity. The transformation from γ-Fe to α-Fe occurs at about 600℃.

γ-Fe and α-Fe co-exists until about 500℃.

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

Diffraction patterns from :[(GaAs)7/(AlAs)3]×100

Pixels are individually addressable, and each pixel has a 4- or 6-bit threshold trim adjustment DAC, which can be set to minimize threshold dispersion across the chip. We demonstrated to discriminate low energy fluorescence X-ray below a detective threshold equalized to 15 keV by scattered X-rays with monochromatic beams at the BL46XU using the PILATUS-I SMD. Diffraction spots are a Bragg reflection peak and its higher orders. In addition, some powder diffraction circles are obtained from an aluminum base plate. The left figures show the result of the threshold of 10 keV, where week scatterings are smeared out

• n the interference background. In the 15 keV threshold result described as the right figures, on the
• ther hand, higher order peaks are clearly seen.

Threshold = 10 keV Threshold = 15 keV

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

PILTUS–I chip

• The PILATUS-I chip with 44 × 78 pixels was fabricated in the

radiation tolerant DMILL 0.8 µm CMOS process, and even fully screened chips showed 5 % defective pixels.

• A subtle design oversight also caused the counters in the pixels to

miscount under some circumstances.

Calibrate ReadbackI

Global Tresh

Treshold correction CS Amp Comp

Bump Pad DOUT AOUT

Gate Rowsel Pixsel Pixsel Colsel

• +

Cal 1.7fF

Analog Block Digital Block

15 bit SR counter

Φ12 Clock Gen Ext Clock Ext/Comp Clock

&

Row Select SR Col Select SR

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

PILATUS-II chip architecture

Rowsel Colsel

ENA DCLK DIN DOUT DCAL AOUT

PILATUS II Chip: 60 cols, 97 rows

CHSEL Row selection Coloumn selection

Global Tresh 6 Bit Latch + DAC CS Amp Comp Bump Pad

DOUT AOUT Rowsel Pixsel Pixsel Pixsel Pixsel Colsel

• +

CAL 1.6fF

20 bit Counter

Pixsel Pixsel

&

PILATUS II Pixel Cell

DCLK ENA

Pulse Shaper

DIN

φ1- Gen φ2

CNT/RO

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

PILATUS II

• A redesigned PILATUS-II readout

chip with 60 × 97 pixels in the UMC 0.25 µm COMS process has been developed to replace the PILATUS-II detector.

• Both of PILATUS I problems have

been overcome in the PILATUS-II chip.

• The yield of ‘good’ chips was

about 35% in the DMILL CMOS process, but even good chips still have around 5 % defective pixels. In the 0.25 mm COMS process,

• n the other hand, the yield of

perfect chips was more than 80%.

> 1 MHz < 10 kHz Countung Yield of chip / wafer Defect pixel / class 1 chip 2.4 ms 6.7 ms Readout time 100 MHz 10 MHz Digital clock 20 bit pseudo- random 15 bit pseudo- random Counter 6 bit DAC 4 bit DAC Threshold adjustment < 100 ns ~ 5 ms Analogue amp-

• ut shape

60 x 97 44 x 78 N of PIxel 172µm x 172 µm 217µm x 217 µm Pixel size UMC 0.25µm radiation tolerant CMOS process DMILL radiation tolerant CMOS process Process Pilatus-II Pilatus-I(SLS06) > 1 MHz < 10 kHz Countung Yield of chip / wafer Defect pixel / class 1 chip 2.4 ms 6.7 ms Readout time 100 MHz 10 MHz Digital clock 20 bit pseudo- random 15 bit pseudo- random Counter 6 bit DAC 4 bit DAC Threshold adjustment < 100 ns ~ 5 ms Analogue amp-

• ut shape

60 x 97 44 x 78 N of PIxel 172µm x 172 µm 217µm x 217 µm Pixel size UMC 0.25µm radiation tolerant CMOS process DMILL radiation tolerant CMOS process Process Pilatus-II Pilatus-I(SLS06) < 10 kHz Countung Yield of chip / wafer Defect pixel / class 1 chip 6.7 ms Readout time 10 MHz Digital clock 15 bit pseudo- random Counter 4 bit DAC Threshold adjustment ~ 5 ms Analogue amp-

• ut shape

44 x 78 N of PIxel 217µm x 217 µm Pixel size DMILL radiation tolerant CMOS process Process Pilatus-I(SLS06) < 10 kHz Countung Yield of chip / wafer Defect pixel / class 1 chip 6.7 ms Readout time 10 MHz Digital clock 15 bit pseudo- random Counter 4 bit DAC Threshold adjustment ~ 5 ms Analogue amp-

• ut shape

44 x 78 N of PIxel 217µm x 217 µm Pixel size DMILL radiation tolerant CMOS process Process Pilatus-I(SLS06) ~ 5 % ~ 30 % 0 % ~ 80 %

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

PILATUS II

• Major improvements have been the speed of the single photon

counting circuit and a much higher yield of working pixels/chip. It achieves > 106 X-rays/s/pixel without counting errors, but which was limited to about 104 X-rays/s/pixel in the PILATUS-I.

8keV X-rays, avg rate of 20 pixels

( )

ns e x a R

x a

113 ' = ⋅ ⋅ =

−

τ

τ

Count Rate capability: ~ 3*106 X-rays/s/pixel = ~ 1010 X-rays/s/cm2 Paralyzable counter:

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

Bump-Bonded Module with 16 chips

• 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 µm. 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 µm in thickness.

• Bump-bonding was performed at the PSI.
• Bump bonding quality

Total : 117 modules 0 defect : 3 0 - 0.01% : 43 0.01 - 0.1% : 30 (including sensor defect)

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

PILATUS II Module

1 Hamamatsu Sensor 16 PILATUS II Chips Bump Bonded at PSI with Automated Bump - Bonding Machine Hybrid from Dyconex Mechanical Support Module Control Board

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

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 µm2 Dynamic Range/pixel: 20 bits Read out time: Tro = 2 ms @ 67 MHz Energy Range: 3 – 30 keV Total Power Consumption: 15 W Frame Rate, PCI RO system: 200 Hz Air cooled, very simple operation Electronic shutter, external synchronisation

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

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.

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

X-ray diffraction at 40 Tesla @ Spring 8

trigger 10 ms exposure 10 ms exposure 1 ms 1 s 1 s

Delay 1.4 ms

magnetic pulse 5.5 ms (40T max)

Magneto-striction of Cobalt-Oxide

Experimental Setup: Timing: Powder Pattern at 20 T:

• J. Narumi et al., J. Synchrotron Rad. 13 271-274 (2006)

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

Comparison of diffraction patterns using CCD and pixel detector at a week diffraction condition (beam intensity decreasing by 3-order magnitude)

ADSC Q210 Pilatus-2

974 × 780 pixel image for Cydidine crystal obtained with a superposition of images taken at the 2 × 8 different positions

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

Comparison of integrated intensities using CCD and pixel detector (Cytidine )

ADSC Q210 Pilatus-2

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

Pixel Detectors for Protein Crystallography

λ θ = × ) sin( 2d

Beam Energy: 5-17.5 keV Intensity: >1012/s Focal spot size: Adjustable to >75 x 30 Divergency: <375 x 70 µrad2 (FWHM) µm2 Crystal rotation

• 30-180 degree for complete data set
• Currently: Discrete rotation, integration
• ver certain rotation angle
• Fine φ−slicing with continuos

sample rotation

Spot size:

• Beam size and divergence
• Mosaicity of the crystal
• Distance sample-detector
• Point spread function of detector

Diffraction data

• reflect crystal symmetry group
• orientation of the crystal-> orientation matrix
• High dynamic range: >104 between strong and weak reflections
• Intensities need to be determined accurately (1%)
• Determination of amplitudes and phases leads

to electron density maps

4

2θ

Resolution:

) sin( 2d

For d=λ=1A 2θ=60o

• Crystallized

Protein X-ray Detector Diffraction pattern Diffracted beam

Beam

Thaumatin (PDB code: 1LXZ) M.W. 22188Da Residues 207a.a.

A major purpose of developing a large area pixel detector is for macromolecular crystallography. The final detector (PILATUS-6M) will be 2463 × 2527 pixels covering 424 mm × 435 mm with 5 × 12 modules.

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

The PILATUS 6M Detector for Protein Crystallography

No of Modules 60 Module size 487 x 195 pixels Detector Size 431 x 448 mm2 No of Pixels 2527 x 2463 pixels (6M) Spatial resolution 0.172 x 0.172 µm2 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) Operation mode Fine φ-slicing

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

Fine φ-slicing Conventional Integration

φ Int

Δφ

Rocking curve Φ Int

Δφ

• short readout-time
• Continuous rotation -> no shutter
• no read-out noise

Fine φ-slicing with the PILATUS-Detector

Angular speed ω, Exposure time t Δφ=t*ω

Integrated intensity

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

Fine-φ sliced data-sets with PILATUS-I

• Insulin crystal, 11.9keV, continuous sample rotation
• 1s exposure, 6.7ms read-out time, 180 deg
• 50 images/deg (0.02o/s)
• Complete data set ~ 9000s, 9000 frames

FWHM=0.12o

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

PILATUS 6M at X06SA

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

PX Data Collection with Pilatus 6M (2/3.5.06)

• “Conventional”, shutter operated crystallography
• Detector vertically not centered
• Ferritin 16 keV (0.8253 Å), Insulin 8keV
• D = 345.9 mm
• ∆ φ = 1°, 60 frames
• 1 s exposure time
• No data correction - Flatfield, trimming, geometrical, parallax,

etc.

• 20 bit data scaled to 16 bit
• processed with XDS / XSCALE

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

Pilatus 6M mar225

R a w D a t a , P r e l i m i n i n a r y E x p e r i m e n t s

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

Summary and outlook

• We have been developing the large area single photon counting

pixel detectors.

• Although PILATUS-I SMD has about 5% defective pixels in the

readout chip, we could study how to operate the pixel detector and how to analyze the data.

• PILATUS-II SMD realizes a desired performance with almost zero

defective pixels and a fast frame rate up to 200 Hz. It has wide application range, and will be commercially available in Oct. 2006.

• PILATUS-6M detector with the 5 × 12 modules will be completed
• soon. Its first test is scheduled in October 2006 at the protein

crystallography beamline X06SA at the SLS.

• A 2M pixel detector with the 3 × 8 modules for small angle scattering

and other applications have been designed and will be fabricated in 2007.

• H. Toyokawa @ JASRI/SPring-8

STD6, Carmal, CA 2006/9/15

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. Suzuki , et al...

JASRI, SPring-8, Japan