MIKRO- I NANO-SYSTEMY W CHEMII I DIAGNOSTYCE BIOMEDYCZNEJ MNS-DIAG PROJEKT KLUCZOWY WSPÓŁFINANSOWANY PRZEZ UNIĘ EUROPEJSKĄ Z EUROPEJSKIEGO FUNDUSZU ROZWOJU REGIONALNEGO; UMOWA Nr. POIG.01.03.01-00-014/08-00 Microflow Fluorometer based on Silicon Photomultiplier Wojciech Kucewicz Katedra Elektroniki AGH on behave of M.Baszczyk, P.Dorosz, S.Głąb, Ł.Mik, M.Sapor
Silicon Photomultiplier The idea appears in the late 90-ties: Photon Detection with High Gain Avalanche Photodiode Arrays S. Vasile, P. Gothoskar, R. Farrell, D. Sdrulla (1998) Silicon avalanche photodiodes on the base of metal-resistor-semiconductor (MRS) structures V. Saveliev, V. Golovin (2000)
Silicon Photomultiplier The Silicon Photomultiplier (SiPM) allows to obtain the intrinsic gain for single photoelectron at the level of 10 6, the value close to that of Photomultipliers. Such a large gain, which confirms the name Photomultiplier, became achievable due to the fact that the SiPM operates in limited Geiger mode.
Silicon Photomultiplier They are operated in limited Geiger mode at 10-20% over breakdown voltage. The Silicon Photomultiplier (SiPM) technique connects arrays of compatible photon counting (Geiger mode) photodiodes together in parallel, each with an integrated quench circuit on a single piece of silicon. An incident photon on any photodiode produces a pulse of current at the sensor output
Silicon Photomultiplier k xi ph V bias > V br V - V or - I I ph x n The total output is the sum of all the individual pulses of current which is proportional t to the number of photodiodes detecting a photon at any moment in time, which in turn is proportional to the incident photon flux or light intensity
Silicon Photomultiplier signal Sensl SiPM diode Bias 31V, Laser 1060nm (12dB; f-100khz, pulsewidth 4ns) range 100, threshold 0.95V( just above 1 avalanche) 100 ns
Silicon Photomultiplier Number of entries 5000 4500 4000 3500 3000 1 photon 2 photons 3 photons 4 photons 2500 2000 1500 1000 500 0 0 10 20 30 40 50 60 70 80 90 100 110 120 ADC Presentation of SiPM signal on histogram. Each peak corresponds to the different number of photons register by SiPM.
Silicon Photomultiplier vs. Photomultiplier Advantages of SiPMs: Small size (chip) Low costs Low bias voltage No sensitive to the magnetic Disadvantages of SiPMs: Thermal generation caused dark count rate PMT SiPM Bias >1kV <100V Magnetic field Yes No Quantum efficiency ~ 40% QE (350nm) 25-65% QE (400nm) Gain typically10 6-10 7 ~ 10 6 Dark current dozens CPS 500 kcps Puls duration dozens ns 15-20 ns Jitter ~ 250 ps ~250 ps Mechanical strength Mała Duża Single photon detection Tak Tak
Silicon Photomultiplier applications Low intensity light detection (single photon level) HEP calorimetry, scintillators Medicine PET (positron emmision tomography) Biology fluorescent markers g Scintillator SiPM
Measurement system trigger signal Agilent 33250 generator gate pulses Picosecond 2600C generator Cuvette holder with specimen GPA amplifier QDC device PC with Labview application excitation filter emission filter
Histograms 250ng/ml 15.6ng/ml 3.9ng/ml 976.6pg/ml Results of measurements for different concentration of sodium fluoresceinate
Alghoritm for signal measurement y 2 y 3 y 4 Method I y k y 1 y 5 x 1 x 2 x 3 x 4 x 5 x 6 x n S 1 x x4 xn x( i) y ( ) 1 x i y2 x( i) i x i x i x 2 1 3 n 1 y k
Alghoritm for signal measurement Method II S N 2 H ( i) i 0 i where: i bin number, H(i) number of entrance N max bin number (for 12-bit ADC = 4095) Comparison of both methods for the same data s S S S 1 2 1 0,7%
Fluorescence measurements of sodium fluoresceinte Kuwetka PMMA1.5 ml z roztworem fluoresceiny w buforze TRIS (PH=8) Dioda LED niebieska S500LLB4GH+ 485 nm /20nm filtr optyczny firmy Biotek 530 nm /25nm filtr optyczny firmy Biotek Kolimator zatrzaskowy WT Technology Model 011 (φ=5mm) Zamontowany na wtyku FC światłowodu o parallel setup perpendicular setup With parallel setup the background light level is higher. The perpendicular setup was recommended for future tests.
Fluorescence measurements of sodium fluoresceinate Comparison of measurements with two different SiPM of Hamamtsu of 1 sqr mm size: S10362-11-050C 400 pixels of 50 μm x 50 μm S10362-11-100C 100 pixels of 100 µm x 100 µm The SiPM with less number of pixels has higher efficiency due to higher fill factor. The SiPM with 100 pixels has been used for futher tests.
Fluorescence measurments of sodium fluoresceinate and resurofin
Fluorescence measurments of sodium fluoresceinate and resurofin Sodium fluoresceinate Resorufin The SiPM is sensitive to sodium fluoresceinate for concentration from tenths of pg/ml The SiPM is sensitive to resurofin for concentation from fraction of ng/ml
Fluorescence measurments of sodium fluoresceinate using LED and Laser 488nm Laser 488nm LED With laser 488nm light source the resolution has incresed up to single pg/ml
ASIC for Silicon Photomultipliers readout In 2010 it has been designed and produced an ASIC - 4 channel front end circuit for SiPM readout 4 channel ASIC in AMS 0,35 µm technology Linearity all 4 channels with range up to 20 registered photons Linearity all 4 channels with range up to 200 registered photons
SiPM gain stabilization An algorithm for SiPM gain stabilization for wide rage of temperature variation was implemented
Measurement setup trigger signal excitation filter emission filter Picosecond 2600C generator Cuvette holder with specimen ASIC + FPGA PC with Labview application ASIC Acquisition system with FPGA and USB connection to the computer FPGA USB
Demonstrator of the 2012 Fluorescence detector based on SiPM and dedicated ASIC Pulse generator for LED diode
Driver and data processing Configuration Data taking The GUI for driving, data taking and data analyzing was designed in LabView enviroment Data processing
First measurements of sodium fluorescinate using demonstrator wrt. QDC
Luminescence measurements of medium flowing through microchannel There was tested 2 size of microchannels 300 μm x 100 μm and 60 μm x 60 μm The blue laser 488 nm has been used as excite light source
Measurements of sodium fluorescinate flowing via 60 μm x 60 μm microchannel Comparison of the measurements results taken with SiPM and PMT via channel of 60 μm x 60 μm. Blue LED. Speed rate 15 μl/min.
Measurements of sodium fluorescinate flowing via 60 μm x 60 μm microchannel Comparison of the measurements results taken with SiPM and PMT via channel of 60 μm x 60 μm. Laser 488 nm. Speed rate 15 μl/min.
Measurements of sodium fluorescinate flowing via 60 μm x 60 μm microchannel K number of noise count N total counts number S1 mean signal value after noise cutting S 1 K N S 1 H ( i i N K ) 1 i K N 2 H ( i) N i 0 i N S2 mean signal value with noise included Only events with photon registration has been taken into account All events has been taken into account but pulse height of noise cases was count as 0
Measurements of sodium fluorescinate flowing via 60 μm x 60 μm microchannel Alghoritm with noise cases included caused incresing of sensitivity up to 10 pg/ml. It doesn t change the curve shape for higher concetrations.
Measurements of sodium fluorescinate flowing via 60 μm x 60 μm microchannel vs. flow rate There is no significant difference of fluorescence light intensity in fuction of flow rate 0,01% /1 µl/min
Conclusions The measuring system leaning on the discrete blocks and SiPM has been created. It has proved opportunity of the measurements system based on SiPM for fluorescent light measurements. There was designed, produced and tests the ASIC for signal readout from the SiPM. The demonstrator of microflow fluorometer was built and preliminary tested. Performed tests confirm, that demonstrator parameters are comparable with professional devices available on the market.
Publications Rok 2010: 1. Ł. Mik, J. Stępień, M. Jastrząb, W. Kucewicz, M. Sapor - System for low intensity fluorescence light measurement based on silicon photomultiplier, ICSES 2010 Proceedings, 7-10 Sept. 2010, p.383-386 2. Ł.Mik, M. Jastrząb, W. Kucewicz, M. Sapor, A. Czermak, B. Sowicki System for Photon Counting with Silicon Photomultiplier, ICSES 2010 Proceedings, 7-10 Sept. 2010, p.439-442 Rok 2011: 1. Jerzy Barszcz, Mateusz Baszczyk, Piotr Dorosz, Wojciech Kucewicz, Maria Sapor Four Channels Data Acquisition System for Silicon Photomultipliers, Elektronika 12/2011 (2011) 28-31 2. Ł. Mik, W.Kucewicz, J. Barszcz, M. Sapor, S. Głąb - Silicon Photomultiplier as Fluorescence Light Detector, Elektronika 12/2011 (2011) 61-65 3. J. Barszcz, M. Baszczyk, P. Dorosz, W. Kucewicz, M. Sapor Four Channels Data Acquisition System for Silicon Photomultipliers, Proceedings of MIXDES 2011 (2011) 690-693 4. Ł. Mik, W. Kucewicz, J. Barszcz, M. Sapor, S. Głąb Silicon Photomultiplier as Fluorescence Light Detector,, Proceedings of MIXDES 2011 (2011) 663-666 Rok 2012: 1. R. Szczypiński, Ł. Mik, J. Kruk, M. Baszczyk, P. Dorosz, S. Głąb, D.G. Pijanowska, W. Kucewicz Fluorescence detection in microfluidics devices Przegląd elektrotechniczny 10b (2012) 88 2. R. Szczypinski, Ł. Mik, J. Kruk, M. Baszczyk, P. Dorosz, S. Głąb, D.G. Pijanowska, W. Kucewicz. - Detekcja fluorescencji w układach mikroprzepływowych. XII Konferencja Naukowa Czujniki Optoelektroniczne i Elektroniczne, Karpacz 27-27 czerwca 2012. 3. Mateusz Baszczyk, Piotr Dorosz, Sebastian Głąb, Wojciech Kucewicz, Łukasz Mik, Maria Sapor Compensation of the Temperature Fluctuations in the Silicon Photomultiplier Measurement System, Elektronika 7 (2012) 64
Signal from SiPM 1 foton 2 fotony 3 fotony 4 fotony
First measurements of sodium fluorescinate using demonstrator wrt. PMT