Kinetic Analysis and Characterization of Epoxy Resins ... - FedOA
Kinetic Analysis and Characterization of Epoxy Resins ... - FedOA
Kinetic Analysis and Characterization of Epoxy Resins ... - FedOA
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Results <strong>and</strong> Discussion 145<br />
ditions.<br />
The best operating conditions for the microwave curing process have been<br />
determined studying the influence above all <strong>of</strong> three parameters:<br />
1. power ;<br />
2. radiation time;<br />
3. mass <strong>of</strong> the sample.<br />
The power <strong>and</strong> time <strong>of</strong> radiation influence the quantity <strong>and</strong> the rate <strong>of</strong> energy<br />
transfer between the oven <strong>and</strong> the sample. While the mass <strong>of</strong> the sample influences<br />
the energy development during the polymerization. In fact initially the temperature<br />
raises exclusively for dielectric heating, but as soon as the temperature<br />
overcomes a critical value, corresponding to the activation <strong>of</strong> curing process, the<br />
thermal pr<strong>of</strong>ile is controlled, above all, by the heat generated by the exothermicity<br />
<strong>of</strong> the reaction itself.<br />
This heat is proportional to the mass <strong>of</strong> the sample <strong>and</strong><br />
depends in a complicated way on the energy flux received from the oven, through<br />
microwave radiation, <strong>and</strong> on the energy exchange with the outer environment.<br />
Only an accurate selection <strong>of</strong> these three factors ensures a complete conversion <strong>of</strong><br />
the sample, avoiding thermal degradation phenomena.<br />
The values <strong>of</strong> microwave cycle parameters <strong>and</strong> reactants quantity corresponding<br />
to the achievement <strong>of</strong> this condition have been determined after several experiments<br />
<strong>and</strong> they are listed in Tables 3.23 <strong>and</strong> 3.24.<br />
In Figure 3.37 the DSC dynamic scan between 0 up to 220 ◦ C with heating rate<br />
<strong>of</strong> 10 ◦ C/min on a fragment <strong>of</strong> epoxy resin microwave cured as reported above is<br />
illustrated.<br />
No residual enthalpy is present, therefore a complete conversion has been reached.<br />
Furthermore the light yellow colour <strong>of</strong> the resulted slab indicates the absence<br />
<strong>of</strong> thermal degradation phenomena. So with the parameters reported in Tables<br />
145