Subject Number : S-16-MS-1059
Support Type : Technical support
Proposal Title (English) : Radical detection of vulcanization of rubber composite by ESR
Username (English) : Aya HARANO1), Alexandra GABLIER2), Pierre ZERLAUTH1)
Affiliation (English) :1) Nihon Michelin Tire co.,ltd., 2) École Supérieure de Physique et de Chimie Industrielles de la ville de Paris.

1. Summary
Time-dependent ESR signals are observed for the rubber composite sample at vulcanization condition of 160degC. The signals suggested the reaction process of curing; providing knowledge on reaction intermediate and its time-dependent change in its comparative quantity.

2. Experimental
Equipment: ESR (Bruker EMX Plus)
Method: temperature variable

3. Results and Discussion
Time-dependent ESR signals are obtained for the rubber composite which was simply composed by synthetic elastomer, sulfur, and accelerator at 160 degC. Two main signals showed below are extracted from the obtained signals.

1) 1st signal: The signal was characterized as BtS· and BtSx·. The characterization was done based on the ESR signal on model compound.

2) 2nd signal: The signals were suggested to be RSx·. It was supported by the fact that i) the signals started to be appeared after the deceleration phase of MCCSC torque, ii) The shape of the signals suggested the coupling with elastomer chain which will be confirmed by the on-going trial of DFT calculation of g-value.

The basic knowledge obtained here will be applied to the further study to see the influence of a change of the amount/ the variety of vulcanization agent on vulcanization process which will give further insight on the new technology of the control of vulcanization.

4. Others
MCCSC: shear test at given temperature (ex. 160 degC). A change of the torque of a sample was which is used as the indication of the progress of vulcanization

AH sincerely express her gratitude to the National Institute for Materials Science for their support in ‘nanotechnology Platform’. AH also acknowledge the dedicated contribution of Alexandra Gablier of ESPCI on this study.

5. Publication/Presentation
Not applicable

6. Patent
Not applicable