The physical properties of microcapsules are largely influenced by the synthesis conditions such as weight ratio of core/shell material, agitation rate, reaction time, and different emulsifier. Different synthesis condition would lead to different property. It is an important issue for application in composites that require self-healing microcapsules possessing rough surface morphology, less adhesion, less core material permeability, appropriate diameter and core content, and adequate shell thickness. The properties of microcapsules influenced by the synthesis conditions were investigated systematically in this article. According to orthographic factorial design, the most influencing factor on microcapsule's yield, core material, average shell thickness and average diameter, are concluded, respectively. The synthesis parameters when the epoxy-containing microcapsules exhibit the optimum properties are concluded: 1.4 : 1 for the weight ratio of core/shell material, 250 rpm for the agitation rate, 3 h for the reaction time and 1.5% content for the emulsifier DBS. The chemical structure of resultant microcapsules is confirmed by FT-IR, and core material of microcapsule exhibits reactivity through DSC measurement. Subsequently, the microcapsules are characterized by SEM, OM, and contact angle experiment so as to provide parameters of microcapsule's physical properties for making binary selfhealing materials. As a result, the resultant microcapsules are suitable for fabricating self-healing materials.
Microcapsules were prepared by in situ polymerization technology with poly(urea-formaldehyde) (PUF)-grafted c-glycidoxypropyltrimethoxy silane (KH560) copolymer as a shell material and dicyclopentadiene (DCPD) as core materials. The aim was to improve the interfacial bond between microcapsules and epoxy matrix in composites through the epoxy functional group in KH560. The microcapsulating mechanism was discussed and the process was explained. The morphology and shell wall thickness of microcapsules were observed by using scanning electron microscopy. The size of microcapsules was measured using optical microscope and the size distribution was investigated based on data sets of at least 200 measurements. The chemical structure and thermal properties of microcapsules were characterized by Fourier transform infrared spectroscopy, X-ray photoelectron spectra, and thermogravimetric analysis. Results indicted that the PUF-graft KH560 microcapsules containing DCPD can be synthesized successfully; the epoxy functional group was grafted on the wall material. The microcapsule size is in the range of 40-190 lm with an average of 125 lm. The wall thickness of microcapsules sample is in the range of 2-5 lm and the core content of microcapsules is about 60%.
Microcapsules containing healing agent have been used to develop the self-healing composites. These microcapsules must possess special properties during the use of composites such as stability in surrounding, appropriate mechanical strength, and lower permeability. A new series of microcapsules containing dicyclopentadiene with chitosan/urea-formaldehyde copolymer as shell materials were synthesized by in situ copolymerization technology. The microencapsulating mechanism was discussed and the process was explained. Also, the factors influencing the preparation of microcapsules were analyzed. The morphology and shell wall thickness of microcapsules were observed by using scanning electron microscopy. The size of microcapsules was measured using optical microscope and the size distribution was investigated based on data sets of at least 200 measurements. The chemical structure and thermal properties of microcapsules were characterized by Fourier transform infrared spectroscopy and thermogravimetric analysis, respectively. The storage stability and isothermal aging experiment of microcapsules were also investigated. Results indicted that the chitosan/urea-formaldehyde microcapsules containing dicyclopentadiene were synthesized successfully; the copolymerization occurred between chitosan and urea-formaldehyde prepolymer. The microcapsule size is in the range of 10-160 lm with an average of 45 lm. The shell thickness of microcapsules is in the range of 1-7 lm and the core content of microcapsules is 67%.
Healing agent microcapsules have been used to realize self-healing for polymeric composites. In this work a novel kind of microcapsules encapsulating ethylenediamine (EDA) with epoxy resin as shell material were prepared by interfacial polymerization technology. The oil phase was epoxy resin prepolymer and carbon tetrachloride, and the water phase was EDA and deionized water. Under the action of emulsifier, a stable water-in-oil emulsion was formed. Then the emulsion was added to dimethyl silicone oil, stirred and dispersed, to prepare microcapsules. In addition, the factors affecting the preparation of microcapsules were studied. In this study, Fourier transform infrared(FTIR) was carried out to demonstrate the chemical structure of ethylenediamine microcapsules. Optical microscope(OM) and scanning electron microscope(SEM) were used to observe the morphology of microcapsules. Thermogravimetric analysis and differential scanning calorimetry were done to investigate the thermal properties of microcapsules. Permeability experiment and isothermal aging test were executed to verify the environment resistance of microcapsules. Results showed that EDA was successfully coated in epoxy resin and the microcapsule size was in the range of 50~630 μm. The synthesized microcapsules were thermally stable below 75 °C and perfect permeability resistance to ethanol solvent.
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