First measurements Investigations
into the Curing of Hysol 9396 using
Differential Scanning Calorimetry
(Tim)
Differential Scanning Calorimetry
• Study how fully-cured Hysol9396 gets after
different cure times and with different cure
temperatures
– Eg. How well cured is it after 1 day at 22C?
– NB. Hysol received March 2010 !
• Measurements
– Dynamic: Measure heat flow into/out of
sample during a temperature ramp (eg 0 to
220C)
• Measures the maximum possible heat
associated with curing exotherm.
– Static: Measure heat flow into /out of
sample at a fixed temperature followed by
dynamic scan.
• Measures heat associated with curing at fixed
temperature.
– By combining both types of measurement
the degree of cure for a given process can
be determined.
Dynamic scan from 0 to 220C
Dynamic Scans
Dynamic Scans
Wright Report
130412_Hysol_1
130416_Hysol_4
130429_Hysol_14
Wright Report
130419_Hysol_7
130423_Hysol_9
130424_Hysol_11
130425_Hysol_12
130426_Hysol_13
Integrated
Peak (J/g)
535.1
525.7
564
584
170
190.7
179.7
51.24
206.5
172.8
Melting Temp Peak Temp Comment
63.3
62.8
47.4
57.2
60.4
104.6
103.6
102.1
103.3
102.4
WL-TR-92-4060: Askins, R; October 1991; pg 35
Un-cured
Un-cured
Un-cured - < 10min after mixing
AL-TR-92-4060: Askins, R; October 1991; pg 35
After 3 days at 22C
After 4 days at 22C
After 1 day at 22C - very strange!
After 1 day at 22C)
After 2 days at 22C
melting!
Isothermal Scans
Isothermal Scans
Wright Report
Temp
66
Hold
75
Iso Heat
450.0
2nd Onset 2nd Heat
94.0
Tot heat Comment
544.0 WL-TR-92-4060: Askins, R; October 1991; pg 35
130412_Hysol_2
66
60
378.6
95.1
72.0
450.6
130419_Hysol_8
66
75
411.8
96.6
98.9
510.7
130416_Hysol_5
82
60
402.4
115.2
69.4
471.8
130423_Hysol_10
82
60
470.0
130416_Hysol_6
93
60
410.5
470.0
126.9
49.3
459.8
Summary
•
Typical heat released in a dynamic scan of un-cured Hysol is 560 ± 25 J/g (5%). This
compares reasonably well with the data from the Wright Laboratory report.
– “CHARACTERIZATION OF EA9396 EPOXY RESIN FOR COMPOSITE REPAIR APPLICATIONS”
For room-temperature cured Hysol (1-4 days), the un-released heat is typically 190J/g
implying that only 66% of the available heat-release has occurred. (WL-TR-92-4060
quotes 170J/g released after 7 day cure at room temperature)
•
Room-temperature cured sample show indications of melting at about 60C
•
There is some degree of correlation between curing time and heat release/re-melt
temperature.
50%
45%
40%
35%
30%
25%
20%
15%
10%
5%
0%
64
63
62
61
60
59
% Heat
Remaining
58
57
56
0
1
2
3
Cure Days at 22C
4
5
Melt Peak Temp
% Heat Remaining
•