scholarly journals In situ poly(melamine-formaldehyde) microencapsulation of diglycidyl ether of bisphenol-A epoxy and pentaerythritol tetrakis(3-mercaptopropionate) for self-healing applications

2022 ◽  
Vol 1217 (1) ◽  
pp. 012017
Author(s):  
H Ghazali ◽  
K Ghazali ◽  
R Yusoff

Abstract In this study, microcapsules as potential candidates for self-healing agents were prepared by in situ polymerisation, taking place in oil-in-water emulsion. Poly(melamine-formaldehyde) is employed as shell material and diglycidyl ether of bisphenol A as polymerisable core materials and Pentaerythritol Tetrakis(3-Mercaptopropionate) as its hardener. The geometry, shell features, size distributions, core content, and the reactivity of the microcapsules were studied by scanning electron microscopy (SEM), optical microscopy (OM), Soxhlet extraction method and differential scanning calorimetry (DSC). Microcapsules with different sizes and distributions were obtained by adjusting the stirring speeds during the preparation stage. From the results, it was established that the spherical microcapsules fabricated using this technique, resulted in satisfactory size and shell structure with shell thickness of less than 2 μm. The microcapsules possess high core content at about 90 wt.% for each size range of microcapsules and it was also observed that the viscosity of the core content decreased at an elevated temperature. The results obtained in this work indicate that these microcapsules possess the characteristics that can be potentially used for self-healing applications.

2016 ◽  
Vol 694 ◽  
pp. 58-63 ◽  
Author(s):  
Hafeez Ullah ◽  
Khairun Azizi Azizli ◽  
Zakaria Man ◽  
Muhammad Irfan Khan

Three different functionalized polydimethylsiloxane based probable self-healing materials were encapsulated by oil-in-water emulsion polymerization melamine-formaldehyde (MF) microcapsules for future applications in self-healing composites systems. The diameter and morphology, thermal properties, and structural analysis of the synthesized microcapsules were determined by scanning electron microscope (SEM), thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FT-IR), and electron dispersive spectroscopy (EDS). The results showed that nature of core material plays an important role in the morphology and thermal stability of the microcapsules.


2008 ◽  
Vol 47-50 ◽  
pp. 286-289 ◽  
Author(s):  
Hai Ping Wang ◽  
Yan Chao Yuan ◽  
Min Zhi Rong ◽  
Ming Qiu Zhang

For purposes of developing a novel self-healing chemistry for polymer composites, melamine-formaldehyde (MF) resin-walled microcapsules containing styrene were prepared by in-situ polymerization in an oil-in-water emulsion. Chemical structure of the microcapsules was identified by Fourier-transform infrared spectroscopy (FTIR) and proton magnetic resonance spectroscopy (1H NMR), respectively. In addition, scanning electron microscope (SEM) and optical microscope (OM) were used to investigate morphology and geometry of the product. The effects of dispersion rate, weight ratio of core to shell and emulsifier concentration were carefully analyzed. It was found that poly(melamine-formaldehyde) (PMF) microcapsules containing styrene were successfully synthesized through the proposed technical route, and their mean diameters fall in the range of 20~71 µm. The rough surface of the microcapsules is composed of agglomerated PMF nanoparticles. Both core content and size of the microcapsule can be adjusted by selecting different processing parameters. The highest loading of styrene in the capsules is about 60% and the emulsifier with lower molecular weight used to result in higher core content. In terms of differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), thermal behavior and storage stability of the capsules were studied. The results indicated that the microcapsules can be handled up to 72 oC.


Author(s):  
Patryk A. Bolimowski ◽  
Ian P. Bond ◽  
Duncan F. Wass

Mechanically and thermally robust microcapsules containing diglycidyl ether bisphenol A-based epoxy resin and a high-boiling-point organic solvent were synthesized in high yield using in situ polymerization of urea and formaldehyde in an oil-in-water emulsion. Microcapsules were characterized in terms of their size and size distribution, shell surface morphology and thermal resistance to the curing cycles of commercially used epoxy polymers. The size distribution of the capsules and characteristics such as shell thickness can be controlled by the specific parameters of microencapsulation, including concentrations of reagents, stirrer speed and sonication. Selected microcapsules, and separated core and shell materials, were analysed using thermogravimetric analysis and differential scanning calorimetry. It is demonstrated that capsules lose minimal 2.5 wt% at temperatures no higher than 120°C. These microcapsules can be applied to self-healing carbon fibre composite structural materials, with preliminary results showing promising performance.


2012 ◽  
Vol 729 ◽  
pp. 205-209
Author(s):  
Anna Czeller ◽  
Tibor Czigány

In this paper, melamin-formaldehyde microcapsules filled with pentaerythritol tetrakis (3-mercaptopropionate) (PETMP) or epoxy were prepared via oil-in-water emulsion polymerization method. Two different routes were chosen from literature, and applied with some changes. The effects of modification of reaction conditions on the resulting capsules were studied. It was found that too low pH value in the emulsion causes burst polymerization of the wall material, without microcapsule formation. When pH was set to 4.5 spherical microcapsules were formed. Optical microscopy was used to evaluate the microcapsules.


2013 ◽  
Vol 800 ◽  
pp. 471-475
Author(s):  
Wang Rui ◽  
Qian Jin Mao ◽  
Qi Dong Liu ◽  
Xiao Yu Ma ◽  
Su Ping Cui ◽  
...  

The self-healing polymer material which was embedded microcapsules possesses the ability to heal cracks automatically. The microcapsules were synthesized by in-situ polymerization in an oil-in-water emulsion with urea and formaldehyde as the raw shell material,and epoxy resin (E-51)/ xylene as the core material. The impact of stirring speed on the morphology and particle size of synthetic microcapsules were discussed by optical microscopy (OM), scanning electron microscopy (SEM), and Fourier-transform infrared spectrometer (FTIR).Microcapsules of 400~1500 um in diameter were produced by appropriate selection of agitation rate in the range of 300~600 r/min.


2020 ◽  
Vol 32 (6) ◽  
pp. 669-680 ◽  
Author(s):  
Yong Sun ◽  
Shugang Wang ◽  
Xiaosu Dong ◽  
Yuntao Liang ◽  
Wei Lu ◽  
...  

Microcapsules containing isophorone diisocyanate were fabricated in oil-in-water emulsion. The emulsification effect of different emulsifiers during the capsule synthesis was systematically investigated by optical microscope. Three kinds of shell materials were discussed to obtain the high core content, smooth-surfaced, and robust capsule by scanning electronic microscope and Fourier transform infrared spectroscopy. Self-healing performance of corresponding self-healing epoxy composites was fully evaluated by accelerated corrosion test and mechanical test. The results demonstrated that high core content and smooth-surfaced capsules with dense composite shell could be synthesized in polyvinyl alcohol emulsion, and the core content of the optimized capsules was determined as 71.3–84.6 wt% at the capsule size from 35 µm to 154 µm. In addition, the optimized capsules had good processing properties and the corresponding self-healing epoxy composites exhibited excellent core release and self-healing performance.


2012 ◽  
Vol 430-432 ◽  
pp. 960-963 ◽  
Author(s):  
Wan Peng Ma ◽  
Wei Zhang ◽  
Yang Zhao ◽  
Le Ping Liao ◽  
Si Jie Wang

Urea-formaldehyde microcapsules containing epoxy resin is a promising material for self-healing design. The microcapsules were prepared by in-situ polymerization in an oil-in-water emulsion. The microcapsule formation process was monitored using optical microscopy. Surface morphology was observed using field emission scanning electron microscopy. The thermal property of microcapsules was characterized using thermogravimetric analysis. The results indicate that microcapsule wall has a rough outer surface and a smooth inner surface. The microcapsule size is controlled by different agitation rates. Microcapsules have a good thermal stability below 157°C.


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