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Studies on the use of nano zinc oxide and modified silica in NR, CR ...

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Chapter 2<br />

2.2.4 Stra<strong>in</strong>–sweep studies<br />

55<br />

The stra<strong>in</strong> sweep measurements <strong>on</strong> unvulcanized samples <strong>and</strong><br />

vulcanizates were c<strong>on</strong>ducted to study <strong>the</strong> rubber–filler <strong>in</strong>teracti<strong>on</strong>. Rubber<br />

process analyzer (RPA 2000–Alpha Technologies) is a purposely <strong>modified</strong><br />

commercial dynamic rheometer. 3 Such <strong>in</strong>strument was <strong>modified</strong> for captur<strong>in</strong>g<br />

stra<strong>in</strong> <strong>and</strong> torque signals, through appropriate s<strong>of</strong>tware. Filled rubber<br />

materials (vulcanized) exhibit str<strong>on</strong>g n<strong>on</strong>–l<strong>in</strong>ear viscoelastic behaviour, <strong>the</strong><br />

well–known Payne effect, i.e., <strong>the</strong> reducti<strong>on</strong> <strong>in</strong> elastic modulus with<br />

<strong>in</strong>creas<strong>in</strong>g stra<strong>in</strong> amplitude. 6 RPA can do stra<strong>in</strong> sweep tests <strong>in</strong> which <strong>the</strong><br />

variati<strong>on</strong> <strong>of</strong> storage modulus (G’), loss modulus (G”) <strong>and</strong> complex modulus<br />

(G*) with <strong>the</strong> change <strong>in</strong> stra<strong>in</strong> amplitude are measured. With respect to its<br />

measur<strong>in</strong>g pr<strong>in</strong>ciple, <strong>the</strong> RPA cavity must be loaded with an excess volume <strong>of</strong><br />

test material. In agreement with ASTM 5289, <strong>the</strong> manufacturers recommend<br />

to load samples <strong>of</strong> about 5.0g i.e. 4.4cm 3 for a st<strong>and</strong>ard filled rubber<br />

compound with a specific gravity <strong>of</strong> 1.14 g/cc. Samples for RPA test<strong>in</strong>g were<br />

c<strong>on</strong>sequently prepared by die cutt<strong>in</strong>g 46 mm diameter disks out <strong>of</strong> around<br />

2mm thick sheets <strong>of</strong> materials. The test<strong>in</strong>g temperature was selected as 100°C;<br />

a temperature below <strong>the</strong> cur<strong>in</strong>g temperature <strong>and</strong> <strong>the</strong> shear stra<strong>in</strong> was varied<br />

from 0.5% to 100% keep<strong>in</strong>g <strong>the</strong> frequency <strong>of</strong> measurements at 0.5 Hz.<br />

For stra<strong>in</strong> sweep measurements <strong>of</strong> cured compounds, uncured<br />

material is <strong>use</strong>d as <strong>the</strong> test sample that is cured to its optimum cure time <strong>in</strong><br />

<strong>the</strong> RPA cavity <strong>and</strong> <strong>the</strong>n <strong>the</strong> stra<strong>in</strong> sweep tests were carried out at 50°C as a<br />

two–stage programme.<br />

2.2.5 Swell<strong>in</strong>g studies<br />

C<strong>on</strong>tributi<strong>on</strong> to <strong>the</strong> re<strong>in</strong>forcement effect arises from molecular<br />

<strong>in</strong>teracti<strong>on</strong> between <strong>the</strong> rubber <strong>and</strong> <strong>the</strong> filler. This <strong>in</strong>teracti<strong>on</strong> leads to an<br />

<strong>in</strong>crease <strong>in</strong> <strong>the</strong> effective degree <strong>of</strong> cross l<strong>in</strong>k<strong>in</strong>g <strong>and</strong> can be evaluated by<br />

equilibrium swell<strong>in</strong>g. The equilibrium swell<strong>in</strong>g analysis <strong>of</strong> rubber vulcanizate

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