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DETERMINATION OF CURE BEHAVIOR OF PHENOLIC RESINS

M. Zeberkiewicz (BChE) and A. Chatterjee


University of Delaware . Center for Composite Materials . Department of Chemical Engineering

BACKGROUND
PHENOLICS
Good strength-to-weight ratio

BARRIERS

PROBLEMS

Commercially, phenolic resins are prepared in water (10~65%) Water evolved during cure (condensation reaction) High water content produces excess pressure during cure Pressure causes DSC Sample Pan to burst Pan Bursting will damage DSC cell


Ability to be co-cured with other resins

Pan Burst due to Internal Pressure


Water resistant and corrosion resistant


Good fire resistance properties


Environmentally friendly

Graph resulting from a pan burst

GOAL
Determination of the degree of cure of phenolic resin using DSC

DIFFERENTIAL SCANNING CALORIMETER


Heat Flow ( W/g )

RESULTS
Phenolic Ramp, -20C to 250C, 10C/min
0.4 0.2 0.0 -0.2 -0.4 -0.6 -0.8 -1.0 0 50 100 150 200 250

REAL-TIME DEGREE OF CURE


1 0.9 0.8

D e g re e o f C u re

0.7 0.6 0.5 0.4 0.3 0.2 0.1 0 0 50 100 150 200 250 300

APPROACH
Using

a lower weight sample Using a larger volume pan

In DSC, the difference in the amount of heat required to increase the temperature of a sample and reference are measured as a function of temperature

Temperature ( C )
180F

Time (min) 160F

130F

Using 2wt% Phencat 382 Catalyst Total Heat of reaction: 208 11 J/g

In In In

300 min, at 180F, degree of cure reaches ~95% 300 min, at 160F, degree of cure reaches ~91% 300 min, at 130F, degree of cure reaches ~41%

2005, University of Delaware, all rights reserved

DETERMINATION OF CURE BEHAVIOR OF PHENOLIC RESINS


(continued) TIME TO REACH DEGREES OF CURE FOR PHENOLIC RESINS
Time to reach 90% Cure
Time (min) 300

TIME TO REACH DEGREES OF CURE FOR PHENOLIC RESINS

CATALYST EFFECT ON GEL AND CURE TIME


wt%P15 0% wt%P382 2% 3% 4% 6% 8% 0% 0.75% 1.50% 2.25% Gel Time 42-50 hr 34- 38 hr 20-30 hr 8-12 hr 5 hr 5 hr 6-10 hr 8-12 hr 27 hr Cure Time 66-72 hr 56 hr 35-42 hr 28 hr 18 hr 20 hr 24 hr 26 hr 35-42 hr

Time to reach 25% Cure 200 150 100 50 0 180F 160F Temperature 130F Tim e (m in)

200 100 0 180F Temperature 160F

0% 0% 0% 0% 3% 2.25% 1.50% 0.75%


Time to reach 50% Cure


100 80 60 40 20 0 180F Temperature 160F Time (min)

Higher temperatures promote shorter cure times

Type of catalyst and amount of catalyst both significantly alter the cure kinetics

CATALYST EFFECT ON VOID FORMATION

CATALYST EFFECT ON VOID FORMATION

CONCLUSIONS

FUTURE WORK
Further testing needs to be done to demonstrate repeatability and validation Development of new catalyst to overcome void formation

1.5 wt% P382, 1.5wt% P15 Many small voids

We have successfully measured the degree of cure for high water content phenolic resin using DSC

ACKNOWLEDGEMENTS
3

wt% P382 voids cure time


Few

3 wt% P15 Many large voids

Long

Faster curing causes larger void formation in the final resin product

The new large volume pan system is very efficient and effective in carrying out the DSC experiments without any pan popping

This work is supported by the Army Research Laboratory through the Composite Materials Research Program. We would like to thank Sadi Islam and Touy Thiravong for their support.

2005, University of Delaware, all rights reserved