1. Find the combined weight of one aluminum pan and one
hermetic lid.
2. Cut one pellet of material into a slice of around 5 mg, weigh it,
and place it inside the pan with the cross section lying on the
bottom.
3. Seal the pan with the hermetic lid and load the pan in the DSC
apparatus.
4. Program the software to measure the sample according to the
following procedure:
(a) Equilibrate the sample temperature at 25
C.
(b) Heat up to 195
C at a rate of 10
C/min. The final
temperature of the heating cycle should be chosen considering the issues explained in Note 4.
(c) Keep the material isothermally for 3 min and then cool to
25
C at the same rate. A second heating cycle might be
needed as described in Note 5.
3.1.2 Rheometry
Rheometry measurements were run under nitrogen atmosphere
and using a 25 mm plate-plate geometry. The results are shown in
Figs. 12 and 13:
1. Set the temperature of the oven at 200
C and allow it to
stabilize.
2. Calibrate the gap and load some material on the bottom plate.
This step should be carried out taking into account the precautions described in Note 6.
3. Allow the temperature to stabilize again and then close the
plates to the measuring gap. Trim the extra material and
lower the gap by an additional 15 μm to get a proper meniscus.
Consider the recommendations in Notes 7 and 8 for proper
gap adjusting.
4. Start the measurement according to the following protocol:
(a) Time sweeps at 1% strain, 1 rad/s, for 300 s.
(b) Frequency sweep at 1% strain, from 628 rad/s to
0.1 rad/s. When choosing the frequency range of interest,
consider the risk of outflow as described in Note 9.
(c) Temperature ramp from the current temperature to 20
C
lower, at 1% strain, 1 rad/s and 5
C/min.
(d) Repeat steps 2 and 3 until complex modulus G∗ exceeds
10
7 Pa.
(e) Temperature ramp from current temperature to 200
C,
at 1% strain, 1 rad/s and 5
C/min.
(f) Frequency sweep at 1% strain, from 628 rad/s to
0.1 rad/s.
80
Andrea Roberto Calore et al.
hermetic lid.
2. Cut one pellet of material into a slice of around 5 mg, weigh it,
and place it inside the pan with the cross section lying on the
bottom.
3. Seal the pan with the hermetic lid and load the pan in the DSC
apparatus.
4. Program the software to measure the sample according to the
following procedure:
(a) Equilibrate the sample temperature at 25
C.
(b) Heat up to 195
C at a rate of 10
C/min. The final
temperature of the heating cycle should be chosen considering the issues explained in Note 4.
(c) Keep the material isothermally for 3 min and then cool to
25
C at the same rate. A second heating cycle might be
needed as described in Note 5.
3.1.2 Rheometry
Rheometry measurements were run under nitrogen atmosphere
and using a 25 mm plate-plate geometry. The results are shown in
Figs. 12 and 13:
1. Set the temperature of the oven at 200
C and allow it to
stabilize.
2. Calibrate the gap and load some material on the bottom plate.
This step should be carried out taking into account the precautions described in Note 6.
3. Allow the temperature to stabilize again and then close the
plates to the measuring gap. Trim the extra material and
lower the gap by an additional 15 μm to get a proper meniscus.
Consider the recommendations in Notes 7 and 8 for proper
gap adjusting.
4. Start the measurement according to the following protocol:
(a) Time sweeps at 1% strain, 1 rad/s, for 300 s.
(b) Frequency sweep at 1% strain, from 628 rad/s to
0.1 rad/s. When choosing the frequency range of interest,
consider the risk of outflow as described in Note 9.
(c) Temperature ramp from the current temperature to 20
C
lower, at 1% strain, 1 rad/s and 5
C/min.
(d) Repeat steps 2 and 3 until complex modulus G∗ exceeds
10
7 Pa.
(e) Temperature ramp from current temperature to 200
C,
at 1% strain, 1 rad/s and 5
C/min.
(f) Frequency sweep at 1% strain, from 628 rad/s to
0.1 rad/s.
80
Andrea Roberto Calore et al.