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IRSENS

Integrated sensing platform for gases and liquids in the near and mid-infrared range
J. Faist, P. Jouy
ETH Zurich

Plenary meeting – Bern – May 30th, 2013

Sensing needs
gas fluid

Medicine (Diagnosis, Monitoring)

Environment (Pollution, Modelling)

Sensing of small molecules (CO, CO2, NxOy, ...)

Sensitive Selective

Portable, Low Power

Infrared Spectroscopy

Semiconductor System
Nano-Tera annual meeting, 30. 5. 2013

IrSens – Jerome Faist

Approach: optical sensing
Laser detector N O

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Project Synopsis: Partners

Combine expertise of 7 Swiss groups: Gas

Sources

Interaction system

Software Detection Benchmarking

Liquid

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

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 (EPFL + industrial partner)
IrSens – Jerome Faist Nano-Tera annual meeting, 30. 5. 2013

Measurements in Gases

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Absorption Signature of CO2 Isotopes

12C16O : 2 13C16O : 2 18O12C16O: 17O12C16O:

Main isotope. indicator for heliobacter pyroli → stomach cancer quantifiy soil exchange processes. tracer for stratospheric air.

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Absorption Signature of CO2 Isotopes

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Gas sensor: block diagram

Source: DFB Quantum Cascade Laser

Interaction system: cylindrical mirror cell

Detection: Quantum Cascade Detector

Goal: all parts have a low production cost in large volume
Compared to “standard” systems: - Replace MCT detector with III-V based quantum cascade detector - Develop a new interaction cell

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Gas sensor: toroidal multipass reflection cell
Large incidence angle for short absorption path

Angle of incidence: 𝜃𝜃=3.103  deg Number of Passes: 29 Pathlength: 232 cm

B. Tuzson, M. Mangold, H. Looser, A. Manninen, L. Emmenegger, Opt. Lett. 38, 257 (2013).

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Gas sensor: toroidal multipass reflection cell
Small incidence angle for long absorption path

Angle of incidence: 𝜃𝜃=1.765  deg Number of Passes: 51 Pathlength: 408 cm

B. Tuzson, M. Mangold, H. Looser, A. Manninen, L. Emmenegger, Opt. Lett. 38, 257 (2013).

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Gas sensor: toroidal cell with «Fringe Killer»
Without absorption mask -> interference, fringes

With absorption mask

A patent was filed protecting the use of an absorption mask in a gas cell for MIR laser spectroscopy.
M. Mangold, B. Tuzson and L. Emmenegger, "Method for reducing fringes in laser spectroscopy measurements using an absorption mask in combination with multi-pass optical cells". Switzerland Patent 01884/12, 2012. IrSens – Jerome Faist Nano-Tera annual meeting, 30. 5. 2013

Quantum cascade detector
Active region and responsivity of QCD

D. Hofstetter, J. Di Francesco, L. Hvozdarara, H.-P. Herzig, M. Beck, Appl. Phys. B 103, 967 (2011).

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Quantum cascade detector
Custom-made preamp for QCD

D. Hofstetter, J. Di Francesco, L. Hvozdarara, H.-P. Herzig, M. Beck, Appl. Phys. B 103, 967 (2011).

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Gas sensor: packaging

Measuring gases live in the exhibition!

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Gas sensor: packaging
Light source: a quantum cascade laser Interaction system: a multipass reflection cell Light detector: a quantum cascade detector

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Ultra-compact CO2 isotope analyzer

Good commercialization potential
13CO 12CO acquisition 2 to 2

- 

Full control on experimental environment, laser operation, and data

isotope ratio measurements

Rel. standard deviation (‰)
- 

- 

Real-time fitting engine (up to 1kHz) Directly linked to HITRAN database

1

0.1 10
0

10

1

10 10 Averaging time (s)
2

3

10

4

Isotope ratio measurement precision of 0.2 ‰.

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Measurements in Liquids

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Measurements in liquids
QCL Source Waveguide

QCD Detector Inlets and mixer Outlet

M  M 

Technological blocks:
M  M 

QCL source, waveguide, QCD detector, microfluidics

Benchmarking of the measurements
Compatible solvent: TCE (tetrachloroethylene) M  Extraction and spectroscopy: ATR and direct detection

M 

Integration
IrSens – Jerome Faist Nano-Tera annual meeting, 30. 5. 2013

Measurements in liquids: benchmarking with FTIR
0.06

0.05

0.04 Absorbance

0.03

0.02

0.01

0 1800 1700 1600 1500 1400 1300 −1 Wavenumber [cm ] 1200 1100 1000

Comparison between spectra of pure cocaine, TCE phase of an extract from saliva spiked with pure cocaine and of an extract of saliva spiked with street cocaine (from the Forensic Science Institute Zurich)

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Measurements in liquids: Si/Ge waveguides
Evanescence interaction:

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Measurements in liquids: waveguide geometries

10 mm

Limit of detection: 50 µg/ml

Limit of detection: 5 µg/ml

Improvements to integrate:

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Measurements in liquids: real microfluidic extraction

Parallel Flow

Merging Drainage

Extraction

Droplet Generation

Parallel Flow

outlet inlet

Saliva PCE Cocaine
IrSens – Jerome Faist Nano-Tera annual meeting, 30. 5. 2013

Measurements in liquids: all integrated system
Cocaine measurement in saliva using the all in one chip:

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Measurements in liquids: status
Real life equivalence Cocaine concentration in saliva Detection limit of our system

After one dose: 500 µg/ml

All integrated system

100 µg/ml

5 µg/ml

Long waveguide-liquid interaction

Legal limit: 20 ng/ml

Integration of reference channel and stabilization to reach ΔI / I = 10-5

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Other developments: VCSEL
Technology development: Wafer-fused VCSELs emitting around 7600 cm-1
AlGaAs/GaAs based material (High refractive index contrast)

InAlGaAs/InP based material (High efficiency for 1200-1600 nm range)

Spectroscopy applications:

HF step detection

Ammonia and methane spectra

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Wafer fused 1310 nm VCSEL performance

10 Gbps @ 20°C, ER=3.5 dB, 231)

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Other developments: APD and SPAD array
Avalanche photo diodes:
Performance (APD/linear mode) Dark current @ 1V reverse bias Active area Breakdown voltage Performance (Geiger mode) DCR @ Ve = 1V Id/Iref @ Ve=3V FWHM Time jitter Excess bias voltage 0 10 60 25 900 4 kHz % ps V Min. 2 4 9 Max 20 40 13 Unit pA µm2 V

Exceptionally good current-voltage characteristics! Single Photon Avalanche Diodes array:

light source

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

Publications this year
M  M  M  M  “Sensing cocaine in saliva with infrared laser spectroscopy”, Kerstin M.-C. Hans, Matthias Müller, Michele Gianella, Ph. Wägli and Markus W. Sigrist, Proc. SPIE 8591, 85910F (2013) “Infrared detection of cocaine in saliva with a one-step extraction” submitted “Low-loss germanium strip waveguides on silicon for the mid-infrared”, Y.-C. Chang, V. Paeder, L. Hvozdara, J.-M. Hartmann, and H. P. Herzig, Optics Letters 37, 2883 (2012). “Cocaine detection by a mid-infrared waveguide integrated with a microfluidic chip” , Y.-C. Chang, P. Wägli, V. Paeder, A. Homsy, L. Hvozdara, P. van der Wal, J. Di Francesco, N. F. de Rooij, and H. Peter Herzig, Lab on a Chip 12, 3020 (2012). “Compact multipass optical cell for laser spectroscopy”, B. Tuzson, M. Mangold, H. Looser, A. Manninen, L. Emmenegger, Opt. Lett. 38, 257 (2013). “Droplet-based liquid-liquid extraction and on-chip IR-waveguide-spectroscopy: detection of cocaine in human saliva”, P. Waegli, PhD manuscript (2012). “A Ge-on-Si Single Photon Avalanche Diode Operating in Geiger Mode at Infrared Wavelengths,” M. Aminian, A. Sammak, L. K. Nanver, and E. Charbon, SPIE Defense, Security and Sensing 2012
IrSens – Jerome Faist Nano-Tera annual meeting, 30. 5. 2013

M  M  M 

Conclusion
M  All integrated gas detection demonstrator M  First combination of QCL with QCD M  State of the art measurements on CO2 isotopes
(13C/12C ratio: 0.6 ‰ accuracy in 1s and 0.1 ‰ in 250s) sensitivity, optimization of the gas cell) Multi gas detection (IrNOX and IrSens II)

M  Improvement of the detection limit (better QCD M  M  Commercialization/industralization M  Integrated microfluidic system for liquid-liquid extraction mounted on a Si/Ge waveguide M  ATR measurements down to 5 µg/ml concentrations M  Preconcentration microfluidic system M  Integration of a reference channel and longer waveguide-liquid interaction M  Development of wafer-fused VCSELs around 7600 cm-1 M  Detection of several species (HF, Ammonia, Methane) M  Characterization of APD with extremely good I-V properties M  Optimization of VCSELs geometry for industrial production M  Characterization of SPADs arrays
IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013

IrSens team
ETH K.Hans, Markus Sigrist M. Beck, B. Hinkov, P. Jouy, J. Faist EPFL E. Kapon, A. Sirbu, V. Yakovlev E. Charbon, P. Keijzer, M.Aminian A.  Homsy, P. Wagli, N. DeRooij, L. Hvozdara, J. Di Francesco, Yu-Chi Chang, H.P Herzig UNINE A. Wirthmueller, D. Hofstetter FHNWS H. Looser, W. Koch EMPA B. Tuzson, J. Jagerska, M. Mangold, L. Emmenegger

IrSens – Jerome Faist

Nano-Tera annual meeting, 30. 5. 2013