CURE MONITORING BY FIBER OPTIC SENSOR

Italian Aerospace Research Center

S.Cantoni, A.Calabr

Outline

Fiber Optic Integrated Sensor Project Fresnel sensor system design Isothermal cure kinetics Comparison with calorimetric kinetic data Future developments

Composites Manufacturing Process Optimization and Control

Manufacturing Technology Analysis
Physical Model

OFF LINE
Optimal Operative Parameters

Correction Actuation

Physical Model Based Control

Real Time Monitoring

Energy, Mass, Momentum Balances Constitutive Equations

ON LINE

Sensors

Real Process

Process Status

Fiber Optic Sensor

Fiber optic sensor offers a very powerful tool to perform remote, on-line, in-situ monitoring of composite manufacturing processes.
Free from electromagnetic interference and characterized by high chemical and high temperature resistance. Readily embedded and its small size makes of it minimally intrusive in the composite structures. Due to the capability of this system to be multiplexed, this approach can provide information from several differently located points within the composite.

Fiber Optic Integrated Embedded Sensor

Integrated
Bragg 1 and Bragg 2 to decouple the effects on the strain measurements due to temperature variations and reticulation
Laser beam Bragg Grating 2 Bragg Grating 1 Fiber optic

Fresnel principle based sensor to measure the global refractive index variation due to temperature changes and polymerization advancements
Curing resin

Fresnel sensor

Principle of Operation
Fiber Optic Sensor

The sensor is based on the Fresnel reflection principle:

Resin

Incident Light Reflected Light

the reflection coefficient R is related to the difference between the resin refractive index nm, the fiber optic refractive index nf and the incidence angle.
2

In the case of a monomode fiber the reflection coefficient R at fiber end-resin interface can be expressed:

nf nm R = n + n m f

Y JOINT RESIN LASER DIODE PHOTO DIODE

A pigtailed DFB laser emitting at 1310nm is used to light a step-index monomode fiber. The back reflected laser beam amplitude is splitted by an Y joint realized by a coupling 1x2 to a pin InGaAs photodiode.

The laser amplitude and the operation wavelength are held constant by a feed back control. The overall size of the fiber is less than 130 m.

Sensor system
Y JOINT RESIN
70C

LASER DIODE

PHOTO DIODE

HEAT PUMP PELTIER CONTROL SYSTEM

PD.curr.

Ref.in FUNCT. GEN. LOCK-IN AMPLIFIER

I.out

DAQ SYSTEM

In order to increase the signal to noise ratio, the use of modulated source is suitable. As a consequence, laser beam is externally amplitude modulated and the signal from the photodiode is filtered by a lock-in amplifier.

Photo diode

Sensor system
Laser diode Y joint

Signal analyzer

Sensor output

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

Laser controller

Fiber optic

Peltier effect heat pump

Temperature controller

Isothermal Sensor Output

Sensor output is a voltage signal I(t)=KPR(t), where K accounts for system losses, lock-in amplifier gain and photo diode sensitivity, P is the power injected by the laser diode and R is the reflection coefficient.
1.20 I, V 1.00 6
I, V 1.00 3 1.20

70 C
0.80 0.60 0.40 0.20 0.00 0 1800 3 1

0.80 0.60 0.40

60 C
2

2
0.20 0.00

Time, s

3600

1800

3600

5400 Time, s

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 fiber diameter is 124 m.

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

Sensor output
A proper normalization able to eliminate the P and K effect is:

PK (R (t ) R 0 ) R (t ) R 0 I = = R PK (R R 0 ) R R0
While the refractive index n shows an increase due to polymerization of the order of 10-2, its possible a linear expansion of R(n)=R(n0)+R(n0)(n-n0)+O(n2).

R (t ) R 0 n(t) n0 = n R = R R0 n n0

Reflection coefficient based conversion

1.0 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0.0 0 1800 3600 5400
2 3 1

1.0 0.9 0.8 0.7 0.6 0.5 0.4

60 C

0.3 0.2 0.1 0.0 0 1800

70 C

Time, s

Time, s 3600

Calorimetric Cure Kinetic

Due to the exothermal character of polymerization reactions, the cure kinetic has been characterized through thermocalorimetric technique by the use of the DSC (Differential Scanning Calorimetry). Isothermal conversion is reported, based on the isothermal reaction heat H
Calorimetric Isothermal Conversion
1 0.9

70

60

50

40 C

DSC

0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1

DSC

H(t) H0 = H H0

0 0 3600 7200 Time, s 10800

The tested resin: Bisphenol A epoxy based resin (Shell Epon 828) and Triethylenetraammine (HY951 Ciba) curing agent. Tg=120C

Lorentz-Lorenz law
The Lorentz-Lorenz law relates the change in the refractive index with the density and polarizability :

n2 1 N = 2 3M n + 2
where N is the Avogadro number, M is the molecular weight of polymer repeat unit and is the permittivity of free space.

Some experimental data (De Boer, R. J. Visser, G. P. Melis, 1992), indicate that polarizability is almost constant during polymerization, i.e.

n = n (

Lorentz-Lorenz law

A simplification of the Lorentz-Lorenz law results in a linear relationship between the refractive index and the density changes during polymerization. In the case under study, the latter approximation leads to an absolute error of the order of 10-5.

n =

n(t) n0 (t) 0 = 0 n n0

Literature experimental data suggested that the relation between the calorimetric conversion and the volumetric shrinkage of a reacting resin is linear. Thus, the volume reduction is proportional to the increase of crosslinks, and therefore to the conversion:

(t) 0 H(t ) H0 = = DSC 0 H H0

Linearity Chain Rationale

I, sensor output
Sensor Design

Direct comparison between Fiber Optic Sensor isothermal data and isothermal calorimetric conversion

R, reflection coefficient
Simplification of Fresnel law

n, refractive index

, density

H, calorimetric conversion
Experimental evidence

Simplification of Lorentz Lorenz law

Calorimetric vs. Fiber Optic Sensor Conversion

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

Future work

Non isothermal cure kinetics

Bragg gratings integration