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Cure Monitoring by Fiber Optic Sensor
Cure Monitoring by Fiber Optic Sensor
S.Cantoni, A.Calabr
Outline
Fiber Optic Integrated Sensor Project Fresnel sensor system design Isothermal cure kinetics Comparison with calorimetric kinetic data Future developments
OFF LINE
Optimal Operative Parameters
Correction Actuation
ON LINE
Sensors
Real Process
Process Status
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 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
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
PD.curr.
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
Temperature controller
70 C
0.80 0.60 0.40 0.20 0.00 0 1800 3 1
60 C
2
2
0.20 0.00
Time, s
3600
1800
3600
5400 Time, s
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
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
60 C
70 C
Time, s
Time, s 3600
70
60
50
40 C
DSC
DSC
H(t) H0 = H H0
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:
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
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