Method for determining optimal degree of vulcanization and...

Electricity: measuring and testing – Impedance – admittance or other quantities representative of... – Lumped type parameters

Reexamination Certificate

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C324S607000, C324S658000

Reexamination Certificate

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06924652

ABSTRACT:
The present invention relates to a method for evaluating the crosslink degree of a vulcanized sample in real time during a vulcanization process or diagnosing the electrical properties of the sample after the completion of the vulcanization process, and then determining an optimal vulcanization time and an optimal content of each constituent gradient of a composition for vulcanization that optimize the properties of the composition according to the vulcanization conditions, for the sake of improving the properties of the vulcanized sample prepared from a polymer by vulcanization at a high temperature.The method for determining an optimal vulcanization time and an optimal content of each constituent gradient of a composition for vulcanization that optimize the properties of the composition according to the vulcanization conditions includes: (a) measuring an impedance spectrum in a specific frequency range in the individual vulcanization condition; (b) approximating the measured impedance spectrum to an equivalent circuit model consisting of resistance and capacitance components; (c) determining a polymer resistance Rp (i.e., a value obtained by subtracting a real part of the impedance measurement at a maximum frequency from a real part of the impedance measurement at a minimum frequency, or the magnitude of a real part of the semicircle in a Nyquist diagram) from the determined parameters; (d) determining, as an optimal end point of vulcanization, a time point at which the increasing rate of the polymer resistance Rp rapidly slows down; and (e) determining the optimal content of each constituent ingredient of the composition for vulcanization when the polymer resistance Rp of the sample completely vulcanized is at its minimum.

REFERENCES:
patent: 4868769 (1989-09-01), Persson
patent: 6502046 (2002-12-01), Yoon et al.
patent: 10-257965 (2000-03-01), None
Magil, R. et al, ‘Process Machinery—Using Real-Time Impedance Measurement to Monitor and Control Rubber Vulcanization,’ Rubber World, pp. 24-28, & 62, Dec., 1999.
Nah, C. et al, ‘Effects of Vulcanization Type and Temperature on Physical Properties of Natural Rubber Compounds,’ Elastomer, vol. 35, No. 3, pp. 173-179, 2000.
Park, B.H. et al, ‘Effect of Various Cross-Linking Types on the Physical Properties in Carbon Black-Filled Natural Rubber Compound,’ Polymer (Korea), vol. 25, No. 1, pp. 63-70, 2001.
J. Macdonald, “Impedance Spectroscopy” Emphasizing Solid Materials and Systems a Wiley Interscience Publication, (1987).

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