PROJEKT KLUCZOWY WSPÓŁFINANSOWANY PRZEZ UNIĘ …. Microflow Fluorometer.pdf · Kolimator...

Microflow Fluorometerbased on Silicon Photomultiplier

MIKRO- I NANO-SYSTEMY W CHEMII I DIAGNOSTYCE BIOMEDYCZNEJ

MNS-DIAGPROJEKT KLUCZOWY WSPÓŁFINANSOWANY PRZEZ UNIĘ EUROPEJSKĄ

Z EUROPEJSKIEGO FUNDUSZU ROZWOJU REGIONALNEGO;UMOWA Nr. POIG.01.03.01-00-014/08-00

Wojciech KucewiczKatedra Elektroniki AGH

on behave of M.Baszczyk, P.Dorosz, S.Głąb, Ł.Mik, M.Sapor

MNSDIAG/SMART FRAME conference on „Micro- and nano- systems technology for modern industrial applications”Warsaw 20-21, February 2013

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)

MNSDIAG/SMART FRAME conference on „Micro- and nano- systems technology for modern industrial applications” Warsaw 20-21, February 2013


The Silicon Photomultiplier (SiPM) allows to obtain the intrinsic gain for single photoelectron at the level of 106, 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 .

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





Vbias > Vbr

x n

t

Iph

k xIph V-Vor - I

The total output is the sum of all the individual pulses of current which is proportional 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

100 ns

Sensl SiPM diodeBias 31V, Laser 1060nm (12dB; f-100kHz, pulsewidth 4ns) range 100, threshold 0.95V( just above 1 avalanche)



0

500

1000

1500

2000

2500

3000

3500

4000

4500

5000

0 10 20 30 40 50 60 70 80 90 100 110 120

ADC

Num

ber o

f ent

ries

Presentation of SiPM signal on histogram. Each peak corresponds to the differentnumber of photons register by SiPM.

1 ph

oton

2 ph

oton

s

3 ph

oton

s

4 ph

oton

s


Silicon Photomultiplier vs. Photomultiplier

Advantages of SiPMs:

• Small size (chip)• Low costs• Low bias voltage• No sensitive to the magnetic

Disadvantages of SiPMs:

• Thermal generationcaused dark count rate

PMT SiPMBias >1kV <100VMagnetic field Yes NoQuantum efficiency ~ 40% QE (350nm) 25-65% QE (400nm)Gain typically106-107 ~ 106

Dark current dozens CPS ≈ 500 kCPSPuls duration dozens ns 15-20 nsJitter ~ 250 ps ~250 psMechanical strength Mała DużaSingle photon detection Tak Tak

Low intensity light detection (single photon level)HEP – calorimetry, scintillatorsMedicine – PET (positron emmision tomography)Biology – fluorescent markers

Silicon Photomultiplier applications

Scintillatorg

SiPM

Picosecond 2600C

generator

Cuvette holderwith

specimen

GPAamplifier

QDC device

PC with Labview

application

excitationfilter

emissionfilter

Agilent33250

generator

trigger signal gate pulses

Measurement system

250ng/ml 15.6ng/ml

3.9ng/ml 976.6pg/ml

Histograms

Results of measurements for different concentration of sodium fluoresceinate

Method I

x1 x2x3 x4 x5 x6 xn

yk

y1

y2y3

y4

y5

2

1

4

3 1

)()()( 211

x

xi

x

xi

x

xik

n

n

yixyixyixS

Alghoritm for signal measurement

N

iiiHS

02 )(

Method II

where: i – bin number, H(i) – number of entranceN – max bin number (for 12-bit ADC = 4095)

Comparison of both methods for the same data

Alghoritm for signal measurement

%7,01

21

SSS

s

Fluorescence measurements of sodium fluoresceinte

Dioda LEDniebieska

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

Kuwetka PMMA1.5 ml z roztworem fluoresceiny w

buforze TRIS (PH=8)

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 μmS10362-11-100C – 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 sodiumfluoresceinate and resurofin



Fluorescence measurments of sodiumfluoresceinate and resurofin

ResorufinSodium fluoresceinate

The SiPM is sensitive to sodium fluoresceinate for concentration from tenths of pg/mlThe SiPM is sensitive to resurofin for concentation from fraction of ng/ml


Fluorescence measurments of sodium fluoresceinate using LED and Laser 488nm

With laser 488nm light source the resolution has incresed up to single pg/ml

LEDLaser 488nm

ASIC for Silicon Photomultipliers readout

In 2010 it has been designed and produced an ASIC - 4 channel front–end circuit for SiPM readout

Linearity all 4 channels with range up to 20 registered photons

4 channel ASIC in AMS 0,35 µm technology


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

Picosecond 2600C

generator

Cuvette holderwith

specimen

ASIC+ FPGA

PC with Labview

application

excitationfilter

emissionfilter

trigger signal


Measurement setup

Acquisition system with FPGA and USB connection to the computer

ASICFPGA

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

MNSDIAG/SMART FRAME conference on „Micro- and nano- systems technology for modern industrial applications”Warsaw 20-21, February 2013Data processing

The GUI for driving, data taking and data analyzing was designed in LabView enviroment

First measurements of sodium fluorescinateusing demonstrator wrt. QDC

Luminescence measurements of medium flowing through microchannel


There was tested 2 size of microchannels300 μm x 100 μm and 60 μm x 60 μm

The blue laser 488 nm has been used as excite light source

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.



N

iiiH

NS

02 )(1

NK

K – number of noise count

N – total counts number

S1 – mean signal value after noise cutting

S2 – mean signal value with noise included

N

KiiiH

KNS )(1

1Only 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



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.

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.383-3862. 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) 28-312. Ł. Mik, W.Kucewicz, J. Barszcz, M. Sapor, S. Głąb - „Silicon Photomultiplier as Fluorescence Light Detector”, Elektronika 12/2011

(2011) 61-653. J. Barszcz, M. Baszczyk, P. Dorosz, W. Kucewicz, M. Sapor– „Four Channels Data Acquisition System for Silicon Photomultipliers”,

Proceedings of MIXDES’2011 (2011) 690-6934. 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) 882. 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

Publications


1 foton

2 fotony

3 fotony

4 fotony

Signal from SiPM

First measurements of sodium fluorescinateusing demonstrator wrt. PMT

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