novel fiber optic sensing architectures …novel fiber optic sensing architectures based on...

NOVEL FIBER OPTIC SENSING ARCHITECTURES BASED ON SENSITIVE

NANOFILMS

Ignacio R. Matias, , Francisco J. Francisco J. ArreguiArregui and Richard O. Clausand Richard O. [email protected] [email protected]

Public University of NavarrePamplona; SPAIN

Nanosonic, IncBlacksburg; VA; USA

www.nanosonic.comwww.unavarra.es

[email protected]

Novel fiber optic sensing architectures based on sensitive nanofilms

SummaryIntroduction to the fiber optic sensor marketNanotechnology and fiber optic sensors?The Electrostatic Self-Assembled Monolayer MethodPossible sensing architectures based on nano-films

Tapered ends Tapered optical fibers Hollow core fibersLong period gratingsOptical fiber gratingsNanoFabry-Perot Cavities

Conclusions


ADVANTAGES

- Small and Lightweight- Possibility of being embeded in composite materials- Passive nature- Large dynamic ranges- Single- & Multi-Point Sensing Configurations- Large wideband- Low attenuation- Multiplexing techniques- EMI immunity

Technology Overview. Advantages


Type of optical fiber sensors

Type of Modulation

Intensity

Interferometric

Polarimetric

Spectroscopic

Physical Magnitude

Voltage/current

Temperature

Radiation

Chemical/gas

Rotation

Strain

Electroagnetic fields

Mechanical

Bending/torsion, velocity, vibration/acceleration,displacemen/location, pressure/acoustics, force

Biomedical

Spatial distribution

Point

Distributed

Quasi-distributedNature oftransduction

Intrinsic

Extrinsic

Technology Overview. Classification

Ignacio R. Matías et al. Fiber optic sensors. Encyclopedia of Sensors. Vol. 7, pp. 163-181.


Technology Overview. Extrinsic sensors

Fluorescence

Laser DopplerVelocimetry

ReflectionScattering

Photoelasticeffects

AbsorptionExternal cavities(EFPI)

MEMSOSA

Encoder PlatesDisks

TotalInternal Reflection

Numerical Aperture

Evanescent

Extrinsic Optical Fiber Sensors

Ignacio R. Matías et al. Fiberoptic sensors. Encyclopedia of Sensors. Vol. 7, pp. 163-181.


Technology Overview. Intrinsic sensors

Fiber Bragg Grattings

(FBG)

Microbend

Fiber Lasers/Doped Fibers

PhotonicCrystalFibers

Distributed/Quasi distributed

Raman

Interferometric

Rayleigh

Blackbody

Intrinsic Optical Fiber

Sensors

Mode Coupling

Michelson

Sagnac

Mach-Zehnder

Ring Resonator

Polarization

Fabry-Perot

Long periodgrattingsMulticore FBG Tilted FBG

Tunable FBG

D-Shaped FBG

Chirped FBG

BandGap Fibers

Bragg Fibers

Index-guiding Micromachined Self-AssemblyIn line

Laser fiber

Ignacio R. Matías et al. Fiberoptic sensors. Encyclopedia of Sensors. Vol. 7, pp. 163-181.


Light Sources

PackagingSpecialtyOptical Fibers

Sensors

Detectors &Interrogators

Fiber Optic Sensing System Key Building Blocks

User InterfaceData Acquisition & Interpretation

Design, Planning andInstallation

Courtesy of Alexis Méndez. MCH Engineering, LLC


Market Drawbacks

• Unfamiliarity with the technology• Conservative/no-risk attitude of some industries• Need for a proven field record• Compatibility with existing equipment• Cost• Availability of trained personnel• Turn-key type systems (total sensing solution)• Lack of standards• Quality, performance, packaging & reliability deficiencies across vendors• Major sensing initiatives likely dominated by wireless

Fiber Optic Market Status

� Fragmented

� Niche markets� Foothold in niche applications� Slow adopting industries� Positive investment environment� Major franchises emerging

Positive and continued steady growth� Important growth in chemical/ bio-detection

Courtesy of David Huff (Oida) Source: Quorex


Source: INTECHNO CONSULTING

Sensors Market Size

19982003

2008

0

10000

20000

30000

40000

50000

60000

Development of the World Market Share of Fiber Optical Sensors until 2008

US $ Million

FOS WORLD MARKET

1998 – U$ 175 M – MKT SHARE (0,54%)2003 – U$ 283 M - MKT SHARE (0,67%)2008 – U$ 1450 M –MKT SHARE (2,87%)

AVERAGE OF ANNUAL GROUTH RATE – 23,5%

SENSORS WORLD MARKET

1998 – U$32,534.0M2003 – U$42,158.4M2008 – U$50,594.3M

AVERAGE OF ANNUAL GROUTH RATE – 4,5%


Applications

Civil (bridges, roads, dams, tunnels)

Transportation (Rail monitoring, Weight in motion, Carriage safety)

Energy Industry (Power plants, Boilers & Steam turbines, Power cables, Turbines, Refineries)

Aerospace (Jet engines , Rocket & propulsion systems,

Fuselages)

Oil & Gas (Reservoir monitoring, downholeP/T sensing, seismic

arrays)

Border security and power line

monitoring

Courtesy of David Huff and Alexis Mendez


Courtesy of David Huff (Oida). Source: Light Wave Venture

Optical Fiber Sensor Market Revenues Breakdown


Optical Fiber Sensor Market Forecast

Courtesy of David Huff (Oida). Source: Light Wave Venture




Conclusions


Nanotechnology and fiber optic sensors?

Nanostructure with a size between molecular and microscopic

layers of subwavelength thickness (botton-up)

Nanotextured surfaces Nanoparticles

Nanotubes

Nanofilm1D

2D

3D


Deposition techniques for sensing coatings in OFSDeposition techniques for sensing coatings in OFS

Sputtering in a radio frequencyplanar magnetron systems

Gel solutions

Langmuir-Blodgett

Layer-by-layer

Nanotechnology and fiber optic sensors?

Electron beam, physical and thermal evaporating

Chemical vapor deposition

Spin, dip coatings




Conclusions


Introduction

1960s: Layer-by-layer adsorption of oppositely charged colloidal particles was first proposed by R. K. Iler R.K. Iler, J. Colloid Interface Sci., 21, 569-594 (1966) “Multilayers of colloidal particles”

1990s: reappearance of works on this topic with Decher and co-workers as the pioneers G. Decher, J.-D. Hong, Makromol. Chem., Macromol. Symp., 46, 321-327 (1991).

Today: Layer-by-Layer Electrostatic Self-Assembly (ESA) is one of the most promising techniques for the deposition of nanostructured tailored materials on complex surfaces

• Possible ESA substrates: metals, plastics, ceramics, oxydes, semiconductors withdifferent sizes and shapes such as prisms, concave or convex surfaces.

• Possible ESA coating materials: metals, semiconductors, polymers, dyes, indicators, quantum dots, enzymes and many others (Au, Pt, Al2O3, Fe3O4, SiO2, TiO2, ZrO2, poly(sodium-4-styrenesulfonate) (PSS), poly(diallydimethyl ammonium chloride) (PDDA), polyacrylic acid (PAA), poly(allylamine hydrochloride) (PAH), poly R-478, poly S-119, Neutral Red, Fluorescein, HPTS, PPV, Prussian Blue, Glucose Oxidase, Silica, Quantum Dots…)


The ESA Method: diverse applications

MICROSPHERES

TEXAS A&M, M. McShane et al.COATINGS ON BIOLOGICAL CELLS

University of Melbourne, F. Caruso et al.

SUPERHYROPHOBIC SURFACESM.I.T., M. F. Rubner et al.

PRISMS LENS

NANOSONIC, INC., R. O. Claus et al.FLEXIBLE SUBSTRATES




Conclusions


Nanostructured coatings onto tapered ends of optical fibers

Glucose sensing

tapered ends

Jesús M. Corres, Anai Sanz, Francisco J. Arregui, Ignacio R. Matías and Joaquín Roca. “Fiber optic glucose sensor based on bionanofilms”. Sensors and Actuators B. Not publiseh yet



Tapered ends Tapered optical fibersHollow core fibersLong period gratingsOptical fiber gratingsNanoFabry-Perot Cavities

Conclusions


Tran

smitt

edPo

wer

(dB)

Relative Humidity (%)

Bilayers (5/div)

Experimental response of a 20m waist diameter TOF-based humidity sensors to RH corresponding to three working points of coating thicknesses: 23, 26 and 62 bilayers

Sensors and Actuators B. Vol.122, pp. 442-449. Mars 2007.

Sensors based on Tapered Optical FibersHumidity sensing. Spectral characterization

TOF


Experimental response to the human breathHumidity response time

compared to a commercial one (Blue box humidity sensor

T12000/6,from Philip Harris)

Sensors based on Tapered Optical Fibers

Humidity sensing. Response time

J. M. Corres, F. J. Arregui and Ignacio R. Matias. “Design of Humidity Sensors based on Tapered Optical Fibers”. IEEE Journal of Lightwave and Technology vol. 24 (11); pp.4329-4336 . Nov. 2006


300 350 400 450 500 550 600 650 700 75080

85

90

95

100

105

110

115

120

125

Wavelength (nm)

Tran

smis

sion

(%)

4 min3 min2 min1 min

0 20 400

50

100

Time (min)

Tran

smis

sion

(AU

) Antibody Injection

Binding of antibody

Sensors based on Tapered Optical FibersGliadin sensing (gluten detection)

Tapered Optical Fiber Biosensor for the Detection of Anti-Gliadin Antibodies” . IEEE Sensors Conference 2007.

CladdingCore

Gliadin Overlay

Anti-Gliadin Antibody

Peroxidase

Antigen

Tapered FiberLight In Light Out

Light Source

200 m Fiberμ

Holder

Spectrometer




Conclusions


Sensors based on Hollow core fibers HCF

-35

-30

-25

-20

-15

-10

-5

0

0 20 40 60 80 100

Number of bilayers

Tran

smitt

ed O

ptic

al P

ower

(dB

)

0 200 400 600 800 1000 1200 1400 1600 1800 2000

Thickness of nanofilm (nm)

led at 1310nmled at 850nm

Spectral characterization

Humidity sensing based on evanescent wave

“Nanofilms on hollow core fiber-based structures: an optical study”. IEEE J. of Light. and Tech. Vol. 24 (5); pp. 2100-2107. May 2006


-20

-50

-45

-40

-35

-30

-25

0 10 20 30 40 50 60 70Bilayer

Tran

smitt

ed P

ower

(dB

)

Polycation

Polyanion54 Bilayers

Time (s)

HC

F tra

nsm

itted

po

wer

(dB)

0 10 20 30 40 50 60 70

Time (s)

HC

F tra

nsm

itted

po

wer

(dB

)

23 Bilayers

0 10 20 30 40 50 60 70

Sensors based on Hollow core fibers

breathing monitoring

Humidity sensing based on evanescent wave

Ignacio R. Matías et al. “Nanofilms onto a hollow core fiber”. Opt. Eng. Letters. Vol. 45

(5); 050503. May 2006


Summary

Introduction to the fiber optic sensor marketNanotechnology and fiber optic sensors?The Electrostatic Self-Assembled Monolayer MethodPossible sensing architectures based on nano-films


Conclusions

Novel fiber optic sensing architectures based on sensitive nanofilmsNanostructured coatings on Long Period Gratings: a pH sensor

LPG overlays

Optical response of one of the attenuation bands of a LPG coatedwith [PAH/PAA] coatings when is submitted to pH changes

J. M. Corres, I. Del Villar, I. R. Matias, F. J. Arregui, Optics Letters, 32 (1), 29, 2007


Summary

Introduction to the fiber optic sensor marketNanotechnology and fiber optic sensors?The Electrostatic Self-Assembled Monolayer MethodPossible sensing architectures based on nano-films


Conclusions


Optical fiber microgratings gratings

Fabrication of Microgratings on the Ends of Standard Optical Fibers by the Electrostatic Self-Assembly Monolayer Process. Optics Letters, vol. 26 (3); pp. 131-133, 2001.


-2

-1

0

1

2

3

4

5

1150 1200 1250 1300 1350 1400 1450 1500 1550 1600 1650Wavelength (nm)

Refle

cted

Opt

ical

Pow

er (d

B)

REFERENCE

SENSING

A

BC

A- PURGED AIRB- 0.6 gr/l DCMC- SATURATION OF DCM

opticalfiber

H H HL L

opticalfiber

HL L

opticalfiber

H H HL L

opticalfiber

HL L

micrograting

EXPERIMENTAL RESULTS -VOLATILE ORGANIC COMPOUND SENSOR DICHLOROMETHANE (DCM)

gratings


-2

-1

0

1

2

3

4

5

1150 1250 1350 1450 1550 1650Wavelength (nm)

Ref

lect

ed O

ptic

al P

ower

(dB

)

Different spectral responsesDifferent spectral responses

Sensor 1Sensor 1

-0,50

0,51

1,52

2,53

3,54

4,55

1150 1250 1350 1450 1550 1650Wavelength (nm)

Ref

lect

ed O

ptic

al P

ower

(dB

)

Sensor 2Sensor 2

gratings

F. J. Arregui, Richard O. Claus, Kristie L. Cooper, Carlos Fdez-Valdivielso and Ignacio R. Matías. “Optical Fiber Gas Sensor Based on Self-Assembled Microgratings”. IEEE Journal of Lightwave Technology, vol. 19 (12); pp. 1932-1937, 2001.


1D PBG with defects others

Refractometer

Optics Letters. 28 (13), pp. 1099-1101, 2003




Conclusions


LED

optical fiberindex

matchinggel

sensingelement

opticalfiber

H

opticalfiber

nanocavity

coupler

Photodetector

nanoFabry-Perots

NFP Cavities. Experimental set-up


125 microns

nanoFabry-Perots


0.6

0.7

0.8

0.9

1.0

1.1

1.2

400 500 600 700 800 900

Wavelength (nm)

Abs

orba

nce

(a. u

.)

pH =6

pH =5

pH =7

pH =8

nanoFabry-Perots

NFP Cavities. pH Sensors


0.5

0.7

0.9

1.1

1.3

1.5

0 5 10 15 20 25Time (minutes)

Abso

rban

ce (a

bsor

banc

e un

its)

pH7

pH5

nanoFabry-Perots



nanoFabry-Perots

-3

-2.5

-2

-1.5

-1

-0.5

0

0 10 20 30 40 50 60Time (min)

Ref

lect

ed o

ptic

al p

ower

(dB

)

pH = 6

pH = 5

pH = 4



-8.0

-7.0

-6.0

-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

400 500 600 700 800 900 1000 1100

Wavelength (nm)

Ref

lect

ed O

ptic

al P

ower

(dB

)

Spectral response to:

11 %RH43 %RH98 %RHAcetoneEthanolDichloromethane

Spectral response to NH3

< 4% of cross-sensitivity to other compounds

5.6 dB with NH3

NFP Cavities. Ammonia sensors

nanoFabry-Perots

D. Galbarra, F. J. Arregui, I. R. Matias and R. O. Claus, Smart Materials and Structures, 14 (4), 2005


-5.0

-4.5

-4.0

-3.5

-3.0

-2.5

-2.0

-1.5

-1.0

-0.5

0.0

0 20 40 60 80 100 120 140 160 180 200Time (minutes)

Ref

lect

ed O

ptic

al P

ower

(dB

)

NH3 NH3 NH3 NH3 NH3 NH3

OFF OFF OFF OFF OFF

1 2 3 4 5 6

Dynamic response of a 25 bilayers sensor to Ammonia

NFP Cavities. Ammonia sensors

nanoFabry-Perots


NFP Cavities. Ammonia sensors nanoFabry-Perots

Recovery time < 4 seconds

-3.0

-2.5

-2.0

-1.5

-1.0

-0.5

0.0

0 5 10 15 20 25 30 35 40

Time (seconds)

Ref

lect

ed O

ptic

al P

ower

(dB

)

Smart Materials and Structures. Vol. 14; pp. 739-744, 2005.


NFP Cavities. Volatile organic compounds sensors[Vap+PAH+/PAA-]

nanoFabry-Perots

-0,4

-0,2

0

0,2

0,4

0,6

0,8

0 5 10 15 20 25Nº layer

Ref

lect

ed o

ptic

al p

ower

(dB

) PAH+(Vap)PAA-

Sensors and Actuators B. Vol. 115 (1); pp. 444-449, 2006


0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

0.45

0.5

450 550 650 750 850 950 1050

Wavelenght (nm)

Abs

orba

nce

(A.U

.)Methanol (125 mmol/l)Ethanol (86 mmol/l)Isopropanol (40 mmol/l)

Absorbance spectra of the sensor after 40 minutes exposure

NFP Cavities. Volatile organic compounds sensors nanoFabry-Perots


Response of the sensor for different methanol concentrations

NFP Cavities. Volatile organic compounds sensors

-3

-2.5

-2

-1.5

-1

-0.5

0

0.5

0 10 20 30 40 50 60

Time (minutes)

Ref

lect

edO

ptic

alpo

wer

(dB

)

31 mmol/l (methanol)62 mmol/l (methanol)125 mmol/l (methanol)

nanoFabry-Perots


-2.5

-2

-1.5

-1

-0.5

0

0.5

0 10 20 30 40 50

Time (minutes)

Ref

lect

edop

tical

pow

er(d

B)

21.5 mmol/l (ethanol)43 mmol/l (ethanol)86 mmol/l (ethanol)

Response of the sensor for different ethanol concentrationsNFP Cavities. Volatile organic compounds sensors nanoFabry-Perots


Comparison between ethanol and methanol

NFP Cavities. Volatile organic compounds sensors

-3

-2,5

-2

-1,5

-1

-0,5

0

0,5

0 20 40 60 80 100

Time (minutes)

Ref

lect

edop

tical

pow

er(d

B) Ethanol (86 mmol/l) Methanol (86 mmol/l)

nanoFabry-Perots


108

109

110

111

112

113

114

115

116

0 20 40 60 80 100 120 140 160 180 200time (min)

Ref

lect

ed o

ptic

al p

ower

(nW

) H2O2 2·10-5H2O2 5·10-5

H2O2 5·10-6 H2O2 10-5

H2O2 5·10-4

H2O2 10-40

0,2

0,4

0,6

0,8

1

1,2

1,4

1,6

1,8

0 20 40 60 80 100 120H2O2 concentration (micromolar)

Slop

e (n

W/m

in)

0

5

10

15

20

25

30

35

40

45

0 20 40 60 80 100 120H2O2 concentration (micromolar)

Res

pons

e tim

e (m

in) Response of the sensor for different concentrations of

hydrogen peroxide at pH 4:

1.- Reflected optical power

2.- Slope of the change in the reflected power

3.- Response time

NFP Cavities. Hydrogen peroxide sensor nanoFabry-Perots


NFP Cavities. Human breathing

nanoFabry-Perots

Sensor and opto-electronic units

Face mask and sensor


NFP Cavities. Human breathing

(a) (b)

(c) (d)nanoFabry-Perots

IEICE Transactions on Electronics, vol. E83-C (3); pp. 360-365, 2000


NFP Cavities. Interrogator system for NFP reflexive sensors

nanoFabry-Perots


nanoFabry-Perots

NFP Cavities. Humidity sensors using silica nano-spheres

Caracterization (AFM)

50 nm SiO2 nanoparticlesContact angle: 5º

Surface: Silica




Conclusions


CONCLUSIONS

• The Layer-by-Layer Electrostatic Self-Assembly Method has been presented as a useful tool for fabricating nano-structured sensing coatings, not only fiber optic sensors.

• These coatings can be deposited on substrates of different shapes: flat, cylindrical or conical

• Different optical fiber sensors have been already experimentally demonstrated (humidity, volatile organic compounds, ammonia, glucose, etc.) and the possible applications of this technique in the sensing field are very promising.

• The sensors have a very fast response time, can operate at room temperature and it is possible to find a suitable architecture depending on the specific application.

• Several different optical fiber structures to fabricate sensors have been proposed: Tapered ends, Tapered optical fibers, Hollow core fibers, Long period gratings, Optical fiber gratings, NanoFabry-Perot Cavities, 1D PBG with defects, etc.). All of them are feasible to be implemented using ESA technique with different sensing properties and final performances.

• It is possible to design specific sensors for specific applications by varying any of the design parameters: materials, thickness, number of bilayers, structures, etc.


ACKNOWLEDGEMENTS

Public University of Navarre

Ignacio Del VillarJesus M. CorresJavier BravoJavier GoicoecheaCarlos RuizCesar ElosuaMiguel AchaerandioManuel Lopez-AmoCandido Bariain

All the people at Nanosonic, Incwww.nanosonic.com

This is the result of the contribution of many people

All the people at Virginia TechFiber & Electro-OpticsRESEARCH CENTER

NOVEL FIBER OPTIC SENSING ARCHITECTURES BASED ON SENSITIVE

NANOFILMS

Ignacio R. Matias, Francisco J. Francisco J. ArreguiArregui and Richard O. Clausand Richard O. [email protected] [email protected]

Public University of NavarrePamplona; SPAIN

Nanosonic, IncBlacksburg; VA; USA

www.nanosonic.comwww.unavarra.es

[email protected]

novel fiber optic sensing architectures …novel fiber optic sensing architectures based on...

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