Abstract

The scattering length of a proton against a polarized neutron depends strongly on the polarization of proton spins (PH). This dependence can be utilized for contrast variation in small angle neutron scattering (SANS). We applied this spin contrast variation technique to a silica-filled SBR rubber specimen, which is widely used for tread rubber of fuel-efficient tires. For realizing high PH, we used dynamic nuclear polarization (DNP) technique, in which large polarization of electron spin at low temperature and high magnetic field is transferred to proton spin by microwave irradiation with a tuned frequency. As this electron spin source, we doped stable radical TEMPO (2,2,6,6-tetramethyl piperidine 1-oxyl) into the rubber sample by use of a vapor sorption technique. For the TEMPO-doped rubber sample, SANS measurements were conducted at PH = −20%, 0%, and +13%, with almost fully polarized neutron beam %) with its wavelength of 6.5±0.6 Å. The SANS profile clearly changed as a function of PH, which can be explained by the PH dependence of the neutron scattering length densities of the main three components (SBR, silica and zinc oxide). By a linear transformation of the profiles obtained at the three different PH values, we successfully determined the partial scattering function of silica, which reflects the aggregation of silica particles.

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