cure monitoring by fiber optic sensor

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    CURE MONITORING BY FIBEROPTIC SENSOR

    S.Cantoni, A.Calabr

    Italian Aerospace Research Center

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    Outline

    Fiber Optic Integrated Sensor Project

    Fresnel sensor system design

    Isothermal cure kinetics

    Comparison with calorimetric kinetic data

    Future developments

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    Composites ManufacturingComposites Manufacturing

    Process Optimization and ControlProcess Optimization and Control

    OFFOFF

    LINELINE

    OptimalOperative

    ParametersONON

    LINELINE

    RealProcess

    Sensors

    Process

    Status

    PhysicalModel Based

    Control

    CorrectionActuation

    ManufacturingTechnologyAnalysis

    Energy, Mass,Momentum Balances

    ConstitutiveEquations

    PhysicalModel

    Real TimeMonitoring

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    Fiber Optic Sensor

    Fiber optic sensor offers a very powerful tool toperform remote, on-line, in-situ monitoring ofcomposite manufacturing processes.

    Free from electromagnetic interference andcharacterized by high chemical and hightemperature resistance.

    Readily embedded and its small size makes of itminimally intrusive in the composite structures.

    Due to the capability of this system to bemultiplexed, this approach can provideinformation from several differently locatedpoints within the composite.

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    Curingresin

    Fiber Optic Integrated Embedded Sensor

    Fiber optic

    Laser beam

    Fresnelsensor

    Bragg

    Grating 2Bragg

    Grating 1

    Integrated

    Bragg 1 and Bragg 2 todecouple the effects on the strainmeasurements due to temperaturevariations and reticulation

    Fresnel principle based sensor tomeasure the global refractiveindex variation due to temperature

    changes and polymerizationadvancements

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    Principle of Operation

    Fiber Optic Sensor

    Incident Light

    Reflected Light

    Resin

    The sensor is based on theFresnel reflection principle:

    the reflection coefficient R isrelated to the differencebetween the resin refractiveindex nm, the fiber optic

    refractive index nf and theincidence angle.

    In the case of a monomode fiberthe reflection coefficient R at fiber

    end-resin interface can beexpressed:

    2

    mf

    mf

    nnnnR

    +=

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    LASER

    DIODE

    Y JOINT

    RESIN

    PHOTO

    DIODE

    A pigtailed DFB laseremitting at 1310nm is usedto light a step-index

    monomode fiber. The backreflected laser beamamplitude is splitted by an Y joint realized by a coupling1x2 to a pin InGaAs

    photodiode.

    The laser amplitude and the operation wavelength are heldconstant by a feed back control. The overall size of the fiber is less

    than 130 m.

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    Sensor system

    In order to increase the signal to noise ratio, the use of modulatedsource is suitable.As a consequence, laser beam is externally amplitude modulated

    and the signal from the photodiode is filtered by a lock-in amplifier.

    70C

    LASER

    DIODE

    Y JOINT

    RESIN

    PHOTO

    DIODE

    FUNCT.

    GEN.LOCK-IN

    AMPLIFIER

    Ref.in

    PD.curr.

    I.out

    DAQSYSTEM

    HEAT PUMP PELTIER

    CONTROL SYSTEM

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    Sensor system

    Peltier effectheat pump

    Temperature controller

    Fiber optic

    Y joint

    Laser diode

    Photo diode

    Laser controller

    Signal analyzer Sensor output

    )t(R)t(KP)t(I =

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    0.00

    0.20

    0.40

    0.60

    0.80

    1.00

    1.20

    0 1800 3600Time, s

    I, V

    12

    3

    4

    5

    6

    0.00

    0.20

    0.40

    0.60

    0.80

    1.00

    1.20

    0 1800 3600 5400

    Time, s

    I, V

    1

    2

    3

    Isothermal Sensor Output

    Sensor output is a voltage signal I(t)=KPR(t)I(t)=KPR(t),

    where K accounts for system losses, lock-in amplifiergain and photo diode sensitivity, P is the powerinjected by the laser diode and R is the reflectioncoefficient.

    7070 CC6060 CC

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    The fiber diameter is 124 m.

    Scanning Electron Microscope Analysis

    The fiber cut induces irregularities of the reflectometer surfaces:as a result, the sensor output I0 may vary at the reaction starting

    The K factor [I(t)=KPR(t)] accounts for the effect ofsuch irregularities on the sensor output

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    Reflection coefficient based conversion

    0.0

    0.1

    0.2

    0.3

    0.4

    0.5

    0.6

    0.7

    0.80.9

    1.0

    0 1800 3600 5400

    Time, s

    3

    2

    1

    0.0

    0.1

    0.2

    0.3

    0.4

    0.5

    0.6

    0.7

    0.80.9

    1.0

    0 1800 3600Time, s

    7070 CC6060 CC

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    Calorimetric Cure Kinetic

    The tested resin: Bisphenol A epoxy based resin (Shell Epon828) and Triethylenetraammine (HY951 Ciba) curing agent.Tg=120C

    Due to the exothermalcharacter of polymerizationreactions, the cure kinetic hasbeen characterized through

    thermocalorimetric techniqueby the use of the DSC(Differential Scanning

    Calorimetry).

    Isothermal conversion isreported, based on theisothermal reaction heat H

    Calorimetric Isothermal Conversion

    0

    0.1

    0.2

    0.3

    0.4

    0.5

    0.6

    0.7

    0.8

    0.9

    1

    0 3600 7200 10800Time, s

    DSC

    40 C506070

    0

    0DSC

    HH

    H)t(H

    =

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    Lorentz-Lorenz law

    The Lorentz-Lorenz law relates the change in the refractive index with

    the density and polarizability :

    where N is the Avogadro number, M is the molecular weight of polymerrepeat unit and is the permittivity of free space.

    =+

    M3

    N

    2n

    1n2

    2

    Some experimental data (De Boer, R. J. Visser, G. P. Melis, 1992), indicate

    that polarizability is almost constant during polymerization, i.e.

    ( )= nn

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    =

    =0

    0

    0

    0n

    )t(

    nn

    n)t(n

    A simplification of the Lorentz-Lorenz law results in a linearrelationship between the refractive index and the densitychanges during polymerization.

    In the case under study, the latter approximation leads to anabsolute error of the order of 10-5.

    Lorentz-Lorenz law

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    Literature experimental data suggested that the relation

    between the calorimetric conversion and the volumetricshrinkage of a reacting resin is linear. Thus, the volumereduction is proportional to the increase of crosslinks, andtherefore to the conversion:

    ( )DSC

    0

    0

    0

    0

    HH

    HtH)t(=

    =

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    Simplification ofFresnel law

    Simplification of

    Lorentz Lorenz law

    Experimental

    evidence

    I, sensoroutput

    R, reflection

    coefficient

    n, refractive

    index , density

    H,

    calorimetricconversion

    SensorDesign

    Linearity Chain Rationale

    Direct comparison between FiberOptic Sensor isothermal data andisothermal calorimetric conversion

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    Calorimetric vs. Fiber Optic Sensor Conversion

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    Conclusion

    A Fiber Optic Sensor able to sense isothermal

    cure kinetic has been developed

    Interpretation of sensor output has been provided

    Comparison with calorimetric kinetic data shows

    the system capability in cure monitoring

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    Future work

    Non isothermal cure kinetics

    Bragg gratings integration