The Use of Thin Film Calorimetry in Profiling Norrish Type I and Norrish Type II Photoinitiators

Transcription

1 The Use of Thin Film Calorimetry in Profiling Norrish Type I and Norrish Type II Photoinitiators Kevin Murray Applied Polymer Systems Stephen Siegel UV Process Supply, Inc. Chicago, United States Celeste Diener

2 Open Test Station

3 TFC-9000

4 Dual Test Station

5 Create Temperate set points

6 Real Time Graphing

7 On Line Test Results

8 Specific Heat (J/gC) Exported Test Results CN97A80(Urethane Acrylate)/IRGACURE 69(%) Trial.0E+06 95nm.0E+06.00E+06 5nm 65nm 75nm 8.00E E+05.00E+05.00E E Time (s) 5nm 95nm 75nm 65nm

9 Specific Heat (J/gC) Exported Test Results EBECRYL 70(Bisphenol-A epoxy diacrylate)/itx(%)/edab(5%) Trial 9.00E E+05 5nm,.9s 7.00E E E+05.00E+05 95nm,.5s 65nm,.s 75nm,.s.00E+05.00E+05.00E E Time (s) 5nm 95nm 75nm 65nm

10 Specific Heat (J/gC) Intensity Study 0-00 Ohm Resistance Trials -5.00E+05.50E+05.00E+05.50E+05.00E+05.50E+05.00E E E Time (s) 00 Ohms_Trial 00 Ohms_Trial 00 Ohms_Trial 00 Ohms_Trial 00 Ohms_Trial 5 90 Ohms_Trial 90 Ohms_Trial 90 Ohms_Trial 90 Ohms_Trial 90 Ohms_Trial 5 80 Ohms_Trial 80 Ohms_Trial 80 Ohms_Trial 80 Ohms_Trial 80 Ohms_Trial 5 70 Ohm_Trial 70 Ohm_Trial 70 Ohm_Trial 70 Ohm_Trial 70 Ohm_Trial 5 60 Ohm Data_Trial 60 Ohm Data_Trial 60 Ohm Data_Trial 60 Ohm Data_Trial 60 Ohm Data_Trial 5 50 Ohm_Trial 50 Ohm_Trial 50 Ohm_Trial 50 Ohm_Trial 50 Ohm_Trial 5 0 Ohm Data_Trial 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 5 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 5 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 5 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 5 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 0 Ohm_Trial 5

11 Time to Peak (s) Power vs. Time to peak Time to Peak vs. mw/cm y = 5.5x -0.6 R = mw/cm

12 Intensity vs. Total heat Intensity Studies_Total Heat Released y = -.76x R = 0.98 Total Heat x Resistance (Ohms)

13 Fast Data Collection First test at 0/8/007 8:6AM - Report at 0/8/007 :AM

14 Norrish Type I Reaction

15 Table : TFC data for the 5nm* LED with the polyester acrylates CN6 Initiator Conc. (wt%) t max (s) Slope c max x0 5 (J/g o C) ITX TPO Irgacure *5nm wavelength did not cure BP/EDAB series

16 Table : TFC data for the 95nm LED with the polyester acrylates CN6 Initiator Conc. (wt%) t max (s) Slope c max x0 5 (J/g o C) BP ITX TPO 0.5 Irgacure

17 Table : TFC data for the 75nm LED with the polyester acrylates CN6 Initiator Conc. (wt%) BP 5 6 ITX TPO 0.5 Irgacure 69 t max (s) Slope c max x (J/g o C)

18 Table : TFC data for the 65nm LED with the polyester acrylate CN6 Initiator Conc. (wt%) t max (s) Slope c max x0 5 (J/g o C) BP ITX TPO Irgacure

19 Table 5: TFC data for the 5nm LED with the Bisphenol-A epoxy diacrylate Ebecryl 70 Initiator Conc. (wt%) t max (s) Slope c max x0 5 (J/g o C) ITX TPO Irgacure

20 Table 6: TFC data for the 95nm LED with the Bisphenol-A epoxy diacrylate Ebecryl 70 Initiator Conc. (wt%) t max (s) Slope c max x0 5 (J/g o C) BP ITX TPO Irgacure

21 Table 7: TFC data for the 75nm LED with the Bisphenol-A epoxy diacrylate Ebecryl 70 Initiator Conc. (wt%) t max (s) Slope c max x0 5 (J/g o C) BP ITX TPO Irgacure

22 Table 8: TFC data for the 65nm LED with the Bisphenol-A epoxy diacrylate Ebecryl 70 Initiator Conc. (wt%) t max (s) Slope c max x0 5 (J/g o C) BP ITX TPO Irgacure

23 Table 9: TFC data for the 5nm LED with the urethane acrylates CN97A80 Initiator Conc. (wt%) t max (s) Slope c max x0 5 (J/g o C) ITX TPO Irgacure

24 Table 0: TFC data for the 95nm LED with the urethane acrylate CN97A80 Initiator Conc. (wt%) t max (s) Slope c max x0 5 (J/g o C) BP ITX TPO Irgacure

25 Table : TFC data for the 75nm LED with the urethane acrylate CN97A80 Initiator Conc. (wt%) t max (s) Slope c max x0 5 (J/g o C) BP ITX TPO Irgacure

26 Table : TFC data for the 65nm LED with the urethane acrylate CN97A80 Initiator Conc. (wt%) t max (s) Slope c max x0 5 (J/g o C) BP ITX TPO Irgacure

27 Conclusion The TFC-9000 is able to measure curability with ease and efficiency LED Curing is viable and achievable with the correct photoinitiators for the wavelength