Conventional and diffracted beam electron microscopy can be used to resolve the ultimate crystallite units in standard and heat treated carbon blacks. They are very sensitive in the detection of small differences in crystallite size and orientation. Combined with x-ray diffraction methods and conventional vulcanizate testing, high resolution electron microscopy appears to be a useful and practical means to study carbon black surface activity. All commercial blacks appear to conform in part to the Heckman and Harling concentric crystallite model. Surface activity appears to be related to the extent of this alignment; the less the tangential orientation of the graphite layer planes to the surface, the greater the surface activity. Heating carbon blacks in an inert atmosphere for varying times and temperatures (850 to 1400° C) causes a gradual depression of surface activity with increasing treatment severity, defined by increases in the size and concentric orientation of surface crystallites. At no time was the effect of carbon black on vulcanizate properties changed significantly by heat treatment without disrupting the initial orientation of surface crystallites. Carbon blacks differ in the rate of change of crystallite orientation in response to heat treatment. The initial degree of crystallinity, porosity, and surface volatile content all appear to affect the rate of crystallite orientation and growth. Increases in average crystallite height, Lc, are a good measure of effects of heat treatment in excellent agreement with changes in surface crystallite size and orientation observed with the electron microscope. Commercial ISAF carbon blacks of varied structure have relatively minor differences in surface crystallite orientation, indicating small differences in surface activity. The higher modulus and treadwear associated with the use of high structure blacks appear to be predominantly a result of the chain structure itself. Further evidence was obtained showing that black structure and surface activity are independent properties each of which can have a significant influence on vulcanizate properties such as modulus, treadwear, and hysteresis.

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Hydrosolution masterbatching (HSMB) imparts excellent dispersion and improved pigment-to-polymer adhesion to carbon and oil masterbatches of poly-butadiene, SBR and blends of these rubbers. Tire tests show HSMB stocks to resist wear slightly better than like stocks mixed in a conventional manner. The HSMB process can be used to produce fully compounded vulcanizable tread stocks in which the stock is discharged continuously from a drying extruder. The dispersion and adhesion advantages of HSMB stocks are also noted in complete masterbatches. HSMB oil, black, and polymer masterbatches usually have higher viscosity, tensile strength, hardness, and dynamic modulus but lower resilience and reduced scorch safety, in comparison with conventionally mixed stock. Carbon black dispersion as revealed by light and electron microscope analysis is excellent. Experiments characterizing carbon gel and development of carbon black dispersion on HSMB stocks (vacuum dried), indicate the total effective molecular contact between elastomer and pigment to be increased, so that, in effect, surface area is increased.

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