In this paper, we discussed the drying behavior of monodispersed polystyrene latex at high temperature with particular attention to the morphological evolution during film formation process. At the beginning of the water evaporation, a skin film with some defects was formed at latex/air interface, water evaporated thereby in a constant rate. During this stage, a drying front advanced from the top film towards the bulk dispersion. Afterwards, most water was lost, and water evaporation rate was less than that of the initial stage. In this case, the whole system became immobile, and another drying front developed from the interior region outside the system. Two distinct boundaries between completely dried region and wet region corresponding to the opposite directions of the second drying front were found if the film peeled from the container bottom surface. Besides, some particular morphologies were found in the completely dried region, which was likely related to preferable coalescence among the particles induced by capillary force due to water evaporation.
Phase inversion emulsification technique is an effective physical method to prepare waterborne dispersions of polymeric resins. In this study, a multi\|hollow epoxy resin sphere was obtained by incomplete phase inversion emulsification. The dynamic morphological evolution of water droplets dispersed in bisphenol. A epoxy resin/emulsifier (a multi\|block copolymer) during phase inversion process was investigated with scanning electron microscopy. It is shown that small discrete water droplets are dispersed in the epoxy resin continuous phase at low water content. In this case, the dynamic coalescence among the small water droplets is ignored. With increasing water content, the dynamic coalescence becomes remarkable and larger water drops are formed by the coalescence among the small water droplets. The larger water drops are randomly distributed within the continuous phase. Meanwhile, some necklace like structures with varied length co\|exist with the small water droplets and larger water drops. Incomplete phase inversion is achieved through the coalescence among the larger water drops, and some small water droplets are entrapped therein. In this case, a kind of multi\|hollow sphere is obtained. While, in some local regions, all the nearest small water droplets coalesce simultaneously to be continuous phase to achieve complete phase inversion, and small discrete waterborne particles are obtained. The dynamic coalescence among the small water droplets dispersed in epoxy resin continuous phase could be analyzed in terms of the improved Smoluchowski equation.
The effects of emulsifier molecular architecture on phase inversion process including the critical water content at phase inversion point as well as the particle size are investigated. It is found that the water content at phase inversion point reaches a maximum when the molar ratio of the hydrophilic component PEG10000 to the hydrophobic component bisphenol A epoxy resin E20 is equal to 1∶1, meanwhile, the particle size reaches a minimum (about 100 nm). From the experimental results, it can be seen that to alter the molecular architecture of the emulsifier is an effective method to control the size of the waterborne particles prepared by phase inversion emulsification technique.
Surfactant template synthesis of mesoporous silica monolith was carried out via modified fast sol gel process. It was easy to obtain crack free silica monolith due to low volume shrinkage during the gelation. The morphology of the titled silica was characterized by transmission electron microscopy and X ray diffraction. The results showed that the pores were worm like and the pore size was about 4 nm. Further nitrogen isothermal absorption experiment indicated that the specific area of the titled material was 391 m 2/g, which was comparable with the reported value 306 m 2/g in literature.
A method for preparing 3D ordered macroporous silicate materials was developed by using the ordered stacking structure of monodispersed polystyrene latex as a template. By using a modified sol\|gel procedure, the ordered template was permeated and filled with silicate, and the title porous materials was formed after removing the template by calcination at high temperature. Moreover, the pores were highly ordered throughout all the sample. After observing the morphological profile of the sample before calcination, it was found that silicate existed in two typical morphologies: monodispersed particles in the cavities and interconnected network within the interstice of the template. The transition morphology was rod\|like formed by the condensation of the silicate monodispersed particles. Two aspects concerning with the template effects of the ordered latex film were emphasized: the polymeric spheres may result in orderly packed holes after calcination, and the dielectric interfacial layer surrounding the polymeric spheres may induce the formation of monodispersed silicate spheres with ordered stacking. Both aspects played important roles in the formation of the highly ordered inorganic porous materials by calcination the gel at high temperature.
In this review, our recent work in phase inversion emulsification (PIE) for polymer (especially epoxy resin) waterborne dispersions is summarized. Based on experimental results about PIE process, the physical model is proposed which can guide the synthesis of the waterborne dispersions such as polymer/nanoparticle composite dispersion. In the presence of a latent curing catalyst, PIE can give a crosslinkable epoxy resin waterborne dispersion. The dispersions can form cured transparent coatings with some unique properties such as UV shielding. They are promising in functional coatings, waterborne resin matrices for composites, and sizing for high performance fibers.
The waterborne dispersions of epoxy resin were prepared by the phase inversion emulsification technique. Rheological behavior and its relationship with the structural change of the systems were studied. It was shown that the concentrated dispersions were highly viscoelastic and pseudoplastic, which was attributed to the formation of a physical network among the waterborne particles via hydrogen bond. The dilute dispersions were Newtonian fluids. The discrete clusters composed of small waterborne particles were found in diluted dispersions. With increasing solid content, there existed a structural transition via percolation through a cluster-cluster aggregation mode to form the physical network, which was qualitatively evidenced by the TEM morphologies.