A Structural Study of an Organogel Investigated by Small-Angle Neutron Scattering and Synchrotron Small-Angle X-ray Scattering

• Published in: The journal of physical chemistry. B 2012-07, Vol.116 (26), p.7739-7745
• Main Authors: Takeno, Hiroyuki, Maehara, Akiko, Yamaguchi, Daisuke, Koizumi, Satoshi
• Format: Article
• Language: English
• Subjects: Crystal structure; Fibers; Gelation; Scattering; Small angle X ray scattering; Sol gel process; Styrene acrylonitrile resins; Synchrotrons
• ISSN: 1520-6106; 1520-5207
• DOI: 10.1021/jp3008514

We investigated structures of 12-hydroxystearic acid (12-HSA) gels in a wide temperature range from the gel to the sol states and the gelation process by means of small-angle neutron scattering (SANS) and time-resolved synchrotron small-angle X-ray scattering (SAXS), respectively. The SANS result shows that the size of the cross section of the crystalline fibers in the gel was not affected much by temperature change, although the density of the fibers decreased with the increase of temperature even in the gel state. The SANS profiles at various temperatures and compositions were well reduced by the product of the volume fraction of the fiber and the square of the scattering contrast. At temperatures above the melting point of the gels obtained from differential scanning calorimeter, the gel turned into a homogeneous solution. The time-resolved small-angle X-ray scattering experiments revealed the gelation process as mentioned below. At the early stage, the scattering behavior did not show any change (induction period). The induction period was longer at higher temperatures. In the second stage, an amorphous precursor appeared as an initial structure of crystalline nucleus. In the next stage, the fiber was developed via crystalline nucleation and growth. In this stage, the fibers grew with keeping the size of the cross section (the radius of gyration R ≅ 82 −84 Å) constant, and finally, the fiber growth was arrested because of gelation.