First measurements Investigations into the Curing of Hysol 9396 using Differential Scanning Calorimetry (Tim)

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Presentation transcript:

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 melting! Dynamic Scans Integrated Peak (J/g) Melting Temp Peak Temp Comment Wright Report 535.1 WL-TR-92-4060: Askins, R; October 1991; pg 35 130412_Hysol_1 525.7 Un-cured 130416_Hysol_4 564 130429_Hysol_14 584 Un-cured - < 10min after mixing 170 AL-TR-92-4060: Askins, R; October 1991; pg 35 130419_Hysol_7 190.7 63.3 104.6 After 3 days at 22C 130423_Hysol_9 179.7 62.8 103.6 After 4 days at 22C 130424_Hysol_11 51.24 47.4 102.1 After 1 day at 22C - very strange! 130425_Hysol_12 206.5 57.2 103.3 After 1 day at 22C) 130426_Hysol_13 172.8 60.4 102.4 After 2 days at 22C melting!

Isothermal Scans Isothermal Scans Temp Hold Iso Heat 2nd Onset 2nd Heat Tot heat Comment Wright Report 66 75 450.0 94.0 544.0 WL-TR-92-4060: Askins, R; October 1991; pg 35 130412_Hysol_2 60 378.6 95.1 72.0 450.6 130419_Hysol_8 411.8 96.6 98.9 510.7 130416_Hysol_5 82 402.4 115.2 69.4 471.8 130423_Hysol_10 470.0 130416_Hysol_6 93 410.5 126.9 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.