Surfactant film characterization

Characterization with XRD, SEM, AFM, and ETA Figure 7.2. Preparation of mesoporous titania gel films by surfactant templating (an example). 

Fig. 3.12. Bicontinuous structure with the surfactant molecules aggregated into connected films characterized by two curvatures of opposite sign [9],...

Because of the importance of surfactants in controlling and modifying the surface tension of fluids, it is appropriate here to describe methods for the measurement of surface tension and surfactant film characterization using the Langmuir trough apparatus. 

The area of colloids, surfactants, and fluid interfaces is large in scope. It encompasses all fluid-fluid and fluid-solid systems in which interfacial properties play a dominant role in determining the behavior of the overall system. Such systems are often characterized by large surface-to-volume ratios (e.g., thin films, sols, and foams) and by the formation of macroscopic assembhes of molecules (e.g., colloids, micelles, vesicles, and Langmuir-Blodgett films). The peculiar properties of the interfaces in such media give rise to these otherwise unlikely (and often inherently unstable) structures. 

Figure 9.4. Characterization of mesoporous Si02 films with cylindrical mesopores (ca. 3nm in diameter) templated using Brij 58 surfactant TEM image a), 2D GISAXS pattern with crystallographic indexation b), and SRSAXS/XRR analysis c).The experimental data in c) thus correspond to a detailed scan along the sz axis in b), using a suitable diffractometer. The films were prepared according to Ref. 39 and analyzed by the methods described therein.

As is known, if one blows air bubbles in pure water, no foam is formed. On the other hand, if a detergent or protein (amphiphile) is present in the system, adsorbed surfactant molecules at the interface produce foam or soap bubble. Foam can be characterized as a coarse dispersion of a gas in a liquid, where the gas is the major phase volume. The foam, or the lamina of liquid, will tend to contract due to its surface tension, and a low surface tension would thus be expected to be a necessary requirement for good foam-forming property. Furthermore, in order to be able to stabilize the lamina, it should be able to maintain slight differences of tension in its different regions. Therefore, it is also clear that a pure liquid, which has constant surface tension, cannot meet this requirement. The stability of such foams or bubbles has been related to monomolecular film structures and stability. For instance, foam stability has been shown to be related to surface elasticity or surface viscosity, qs, besides other interfacial forces. 

Many reports are available where the cationic surfactant CTAB has been used to prepare gold nanoparticles [127-129]. Giustini et al. [130] have characterized the quaternary w/o micro emulsion of CTAB/n-pentanol/ n-hexane/water. Some salient features of CTAB/co-surfactant/alkane/water system are (1) formation of nearly spherical droplets in the L2 region (a liquid isotropic phase formed by disconnected aqueous domains dispersed in a continuous organic bulk) stabilized by a surfactant/co-surfactant interfacial film. (2) With an increase in water content, L2 is followed up to the water solubilization failure, without any transition to bicontinuous structure, and (3) at low Wo, the droplet radius is smaller than R° (spontaneous radius of curvature of the interfacial film) but when the droplet radius tends to become larger than R° (i.e., increasing Wo), the microemulsion phase separates into a Winsor II system. 

Transmission electron microscopy (TEM) has been an underutilized yet valuable too in particle size characterization of MC particles in LB films. Monolayer films of trioctylphosphine oxide-capped CdSe (18), spread as a monolayer on an aqueous subphase, were transferred to a TEM grid. A close-packed hexagonal arrangement of 5.3-nm (cr —4%) crystallites was found. TEM images were also obtained for HMP-stabilized CdS incorporated in BeH/octadecylamine films (79) and for CdS formed under an amine-based surfactant monolayer and transferred to a TEM grid (14). In one study, direct viewing of CdS and CdSe particles made from Cd2+-FA films on TEM grids was not possible due to poor phase contrast between the particles and the film (30). Diffraction patterns were observed, however, that were consistent with crystalline (3-CdS or CdSe. Approximately spherical particles of CdSe could... 

Description of the different mimetic systems will be the starting point of the presentation (Sect. 2). Preparation and characterization of monolayers (Langmuir films), Langmuir-Blodgett (LB) films, self-assembled (SA) mono-layers and multilayers, aqueous micelles, reversed micelles, microemulsions, surfactant vesicles, polymerized vesicles, polymeric vesicles, tubules, rods and related SA structures, bilayer lipid membranes (BLMs), cast multibilayers, polymers, polymeric membranes, and other systems will be delineated in sufficient detail to enable the neophyte to utilize these systems. Ample references will be provided to primary and secondary sources. 

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