DeterminationCure_Poster05

8/13/2019 DeterminationCure_Poster05

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2005, University of Delaware, all rights reserved

Determination o f the

degree of cure ofphenolic resin using DSC

BACKGROUND

DETERMINATION OF CURE BEHAVIOR OF PHENOLIC RESINS

M. Zeberkiewicz (BChE) and A. Chatterjee

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

RESULTS

Phenol ic Ramp, -20C to 250C, 10C/min

-1.0

-0.8

-0.6

-0.4

-0.2

0.0

0.2

0.4

0 50 100 150 200 250

Temperature ( C )

HeatFlow(W/g)

Using 2wt% Phencat 382 Catalyst

Total Heat of reaction: 208 11 J/g

Pan Burst due to Internal Pressure

PHENOLICS

Good strength-to-weight ratio

Water resistant and corrosion resistant

Good fire resistance properties

Ability to be co-cured with other resins

Environmentally friendly

APPROACH

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

BARRIERS

GOAL

Graph resulting from a pan burst

Using a lower weight sample

Using a larger volume pan

DIFFERENTIAL SCANNING

CALORIMETER

In DSC, the difference in the amount of

heat required to increase the temperature

of a sample and reference are measuredas a function of temperature

PROBLEMS

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

0 50 100 150 200 250 300

Time (min)

Degreeo

fCure

180F 160F 130F

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

In 300 min, at 130F, degree of cure reaches ~41%

REAL-TIME DEGREE OF CURE

8/13/2019 DeterminationCure_Poster05

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2005, University of Delaware, all rights reserved

Time to reach 50% Cure

0

20

40

60

80

100

180F 160F

Temperature

Time(min)


0

100

200

300

180F 160F

Temperature

Time(min)

CONCLUSIONS FUTURE WORK

ACKNOWLEDGEMENTS

We would like to thank Sadi Islam and Touy

Thiravong for their support.

1.5 wt% P382, 1.5wt% P15

Many small voids

3 wt% P15

Many large voids

Further testing needs to be done to

demonstrate repeatability and validation

Development of new catalyst to overcome

void formation

TIME TO REACH DEGREES OF CURE

FOR PHENOLIC RESINS


0

50100

150200

180F 160F 130F

Temperature

T

ime(min)

This work is supported by the Army Research

Laboratory through the Composite Materials

Research Program.

We have successfully measured the

degree of cure for high water content

phenolic resin using DSC

The new large volume pan system is

very efficient and effective in

carrying out the DSC experiments

without any pan poppingFaster curing causes larger

void formation in the final resin product

TIME TO REACH DEGREES OF CURE

FOR PHENOLIC RESINS

Higher temperatures promote

shorter cure times

CATALYST EFFECT ON GEL

AND CURE TIME

wt%P15 wt%P382 Gel Time Cure Time

0% 2% 42-50 hr 66-72 hr

0% 3% 34- 38 hr 56 hr

0% 4% 20-30 hr 35-42 hr

0% 6% 8-12 hr 28 hr

0% 8% 5 hr 18 hr

3% 0% 5 hr 20 hr

2.25% 0.75% 6-10 hr 24 hr

1.50% 1.50% 8-12 hr 26 hr

0.75% 2.25% 27 hr 35-42 hr

Type of catalyst and amount of catalyst both

significantly alter the cure kinetics

CATALYST EFFECT ON

VOID FORMATION

3 wt% P382

Few voids

Long cure time

CATALYST EFFECT ON

VOID FORMATION

DETERMINATION OF CURE BEHAVIOR OF PHENOLIC RESINS(continued)

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DeterminationCure_Poster05