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RTD Project IRSENS
Integrated sensing platform for gases and
liquids in the near and mid-infrared range


               Y. Bonetti, J. Faist

               ETH Zurich




          Plenary meeting – Bern – May 12, 2011
                                                  IrSens
Project Synopsis: Needs
gas
                                                                fluid
                                               Medicine
                                               (Diagnosis, Monitoring)



                            Sensing of small
                            molecules (CO,
  Environment
  (Pollution, Modelling)    CO2, NxOy, ...)


       Sensitive                                  Portable,
                           Selective              Low Power


       Infrared Spectroscopy           Semiconductor System


                                                                         IrSens
Approach: optical sensing

Laser                  detector
                                  N   O




                                          IrSens
holistic approach

  Gas




          QCL,                    QCD,
                 Electronics
         VCSEL                 SiGe CMOS




Liquid                                     Yes/No
                                             %




                                                    IrSens
Pilot/focus applications

Gas: CO2 isotope ratios, e.g for plant
respiration monitoring – environment

Liquid: Cocaine in saliva detection
(presence yes/no) – traffic security

Platform: develop tools and techniques
  Collaboration with industry started

                                         IrSens
Measurements in Gases




                        IrSens
Schematic of the VCSEL gas-
sensing demonstrator (TDLS)
            Collaboration with an industry
             in collaboration with IR Microsystems / Leister




                                                               IrSens
Cylindrical Multipath Gas Cell

                     20*20*5 cm3




                               IrSens
Benchmarking
Instrumentation benchmarked with different techniques:
- Direct Absorption (DA)
- Wavelength Modulation (WM)                      - Prototype cell
- PhotoAcoustics (PA)                             - wrong QC laser!




Technique            DA            WM             PA                Picarro (CRDS
                     (NanoTera)    (NanoTera)     (NanoTera)        reference)
1s precision (‰)     0.47          0.75           58.8              0.67
best precision (‰)   0.06 (200s)   0.05 (3000s)   0.65 (8000s)      0.1 (300s)


                                                               see poster!
                                                                                 IrSens
Also software!!
full hardware control
data acquisition and processing:
  - real-time fitting module based
  - on Hitran database
measurement automation




                                       IrSens
Measurements in Liquids




                          IrSens
Benchmarking with ATR-
                  Spectroscopy




best spectral
range for
Cocaine in H2O
around 1730/cm
→ sources and
detector design



                                       IrSens
QCL 1721 cm-1 measurements




●
  Strong increase in signal during drying, as expected
●
  Limit of detection around 20 µg/ml
                                                         see poster!
                                                               IrSens
Microfluidic Cell

Source
                               Detector
                 Waveguide


              Inlets and
              Mixer
                      Outlet




                                          IrSens
Transmission through
              waveguide at 6µm see poster!
            Waveguide
QCL




ZnSe lens

      Detector          total transmission
                        through 9mm*5µm
                        waveguide: 4 %

                           IMT
                           Institut de microtechnique   IrSens
Microfluidic Sample Preparation
                    for IR-Detection  see poster!
Problem                        µ-flu. requirements Answer

                               low-cost materials and            rapid prototyping of
disposable chips
                               fabrication process               UV-glue

                               transfer to IR-transparent
mid-IR absorption of water                                       liquid-liquid extraction
                               solvent

IR-transp. organic solvents    chemical compatibility of
                                                                 compatibility tests
used for extraction            chip to solvents

aqueous and organic solvents   handling of multiphase            adjusting wetting
on chip                        flows                             behavior of UV-glue

                               materials with high
absorption of analytes                                           absorption tests
                               recovery rate

                               improvement of liquid-            droplet generation &
fast sample preparation
                               liquid extraction                 separation


                                                 IMT
                                                 Institut de microtechnique                 IrSens
Microfluidic Sample Preparation
         for IR-Detection




               fluid mixing parameters need good control


               IMT
               Institut de microtechnique             IrSens
Support workpackages:
Sources:
           Vertical cavity surface emitting lasers (EPFL)
           Quantum Cascade Lasers (ETHZ)


Detectors:
           Quantum Cascade detectors (UNINE)
           Ge/Si SPADs (EPFL)




                                                            IrSens
Low dissipation, cw QC lasers
2311cm-1     1730cm-1



              1.2W




                         see poster!


                                 IrSens
Detectors:
Quantum cascade detectors,
    SiGe CMOS SPAD




                             IrSens
Ge on Si diode test I-V data




low voltage data for diodes with   Breakdown near -40V
sizes of 1x1, 1x20, and 40x40      (criterion of 1 µA)
micrometer
good material for a detector @ 1.55µm

                                                         IrSens
Quantum cascade detector




Detectivity 5*108 jones (175K, 2300/cm) and
  1.5*107 jones (250K, 1700/cm)
Cold aperture, NTC, black inner side

                                              IrSens
Custom-made QCD preamplifier




          1kHz                    1MHz          Footprint 4 x 4 cm2

• Observed 58 dB of gain in 100mV/nA configuration
• Roughly 25 times more gain than with commercial solution (PA-
9-70 from Judson)
• Almost identically low noise as commercial solution

                                                               IrSens
Achievements

          Near-IR gas system (VCSEL):
               – Industrialization in progress




                                                     Readiness
Novelty




          Mid-IR gas
               – Already reached state of the art
          Mid-IR liquid
               – Key building blocks are validated
               – New detectors & lasers



                                                                 IrSens
IrSens team
ETH                                      UNINE
K.Hans, M. Sigrist                       D. Hofstetter
Y. Bonetti, M. Beck, R. Terazzi,         J. DiFrancesco
EPFL                                      FHNWS
E. Kapon, A. Sirbu                        H. Looser
E. Charbon, M.Aminian
A.Homsy, N. DeRooij,                 EMPA
L. Hvozdara, Y-C.Chang, H.P Herzig   B. Tuzson, A. Manninen, L. Emmenegger




                                                                       IrSens

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Irsens

  • 1. RTD Project IRSENS Integrated sensing platform for gases and liquids in the near and mid-infrared range Y. Bonetti, J. Faist ETH Zurich Plenary meeting – Bern – May 12, 2011 IrSens
  • 2. Project Synopsis: Needs gas fluid Medicine (Diagnosis, Monitoring) Sensing of small molecules (CO, Environment (Pollution, Modelling) CO2, NxOy, ...) Sensitive Portable, Selective Low Power Infrared Spectroscopy Semiconductor System IrSens
  • 3. Approach: optical sensing Laser detector N O IrSens
  • 4. holistic approach Gas QCL, QCD, Electronics VCSEL SiGe CMOS Liquid Yes/No % IrSens
  • 5. Pilot/focus applications Gas: CO2 isotope ratios, e.g for plant respiration monitoring – environment Liquid: Cocaine in saliva detection (presence yes/no) – traffic security Platform: develop tools and techniques Collaboration with industry started IrSens
  • 7. Schematic of the VCSEL gas- sensing demonstrator (TDLS) Collaboration with an industry in collaboration with IR Microsystems / Leister IrSens
  • 8. Cylindrical Multipath Gas Cell 20*20*5 cm3 IrSens
  • 9. Benchmarking Instrumentation benchmarked with different techniques: - Direct Absorption (DA) - Wavelength Modulation (WM) - Prototype cell - PhotoAcoustics (PA) - wrong QC laser! Technique DA WM PA Picarro (CRDS (NanoTera) (NanoTera) (NanoTera) reference) 1s precision (‰) 0.47 0.75 58.8 0.67 best precision (‰) 0.06 (200s) 0.05 (3000s) 0.65 (8000s) 0.1 (300s) see poster! IrSens
  • 10. Also software!! full hardware control data acquisition and processing: - real-time fitting module based - on Hitran database measurement automation IrSens
  • 12. Benchmarking with ATR- Spectroscopy best spectral range for Cocaine in H2O around 1730/cm → sources and detector design IrSens
  • 13. QCL 1721 cm-1 measurements ● Strong increase in signal during drying, as expected ● Limit of detection around 20 µg/ml see poster! IrSens
  • 14. Microfluidic Cell Source Detector Waveguide Inlets and Mixer Outlet IrSens
  • 15. Transmission through waveguide at 6µm see poster! Waveguide QCL ZnSe lens Detector total transmission through 9mm*5µm waveguide: 4 % IMT Institut de microtechnique IrSens
  • 16. Microfluidic Sample Preparation for IR-Detection see poster! Problem µ-flu. requirements Answer low-cost materials and rapid prototyping of disposable chips fabrication process UV-glue transfer to IR-transparent mid-IR absorption of water liquid-liquid extraction solvent IR-transp. organic solvents chemical compatibility of compatibility tests used for extraction chip to solvents aqueous and organic solvents handling of multiphase adjusting wetting on chip flows behavior of UV-glue materials with high absorption of analytes absorption tests recovery rate improvement of liquid- droplet generation & fast sample preparation liquid extraction separation IMT Institut de microtechnique IrSens
  • 17. Microfluidic Sample Preparation for IR-Detection fluid mixing parameters need good control IMT Institut de microtechnique IrSens
  • 18. Support workpackages: Sources: Vertical cavity surface emitting lasers (EPFL) Quantum Cascade Lasers (ETHZ) Detectors: Quantum Cascade detectors (UNINE) Ge/Si SPADs (EPFL) IrSens
  • 19. Low dissipation, cw QC lasers 2311cm-1 1730cm-1 1.2W see poster! IrSens
  • 20. Detectors: Quantum cascade detectors, SiGe CMOS SPAD IrSens
  • 21. Ge on Si diode test I-V data low voltage data for diodes with Breakdown near -40V sizes of 1x1, 1x20, and 40x40 (criterion of 1 µA) micrometer good material for a detector @ 1.55µm IrSens
  • 22. Quantum cascade detector Detectivity 5*108 jones (175K, 2300/cm) and 1.5*107 jones (250K, 1700/cm) Cold aperture, NTC, black inner side IrSens
  • 23. Custom-made QCD preamplifier 1kHz 1MHz Footprint 4 x 4 cm2 • Observed 58 dB of gain in 100mV/nA configuration • Roughly 25 times more gain than with commercial solution (PA- 9-70 from Judson) • Almost identically low noise as commercial solution IrSens
  • 24. Achievements Near-IR gas system (VCSEL): – Industrialization in progress Readiness Novelty Mid-IR gas – Already reached state of the art Mid-IR liquid – Key building blocks are validated – New detectors & lasers IrSens
  • 25. IrSens team ETH UNINE K.Hans, M. Sigrist D. Hofstetter Y. Bonetti, M. Beck, R. Terazzi, J. DiFrancesco EPFL FHNWS E. Kapon, A. Sirbu H. Looser E. Charbon, M.Aminian A.Homsy, N. DeRooij, EMPA L. Hvozdara, Y-C.Chang, H.P Herzig B. Tuzson, A. Manninen, L. Emmenegger IrSens