Title:
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Microcapsules with liquid cores and solid shells for pressure release applications
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The encapsulation of one material by another, to form core-shell particles, has many
applications: principally the containment, protection, and distribution of an active material.
This thesis describes the development of core-shell particles with liquid cores and solid shells
of tunable thickness.
Two main systems are studied. Firstly, polydimethylsiloxane (PDMS) emulsions, or microgels
if cross-linked, are employed as templates for the formation of solid shells. The templates
are prepared by a surfactant-free emulsion polymerization of dimethyldiethoxysilane
(DMDES) that allows monodisperse emulsions to spontaneously form, subject to appropriate
monomer concentrations. The viscosity of the microgel is controlled by variation of the
cross-linking component's concentration. Silica shells were grown upon silica-skinned templates
in a seeded growth process through slow addition of tetraethoxysilane (TEOS) under
basic and ethanolic conditions. Solid silica-silicone composite shells were formed, in the
absence of ethanol, through condensation of TEOS and DMDES. Shell thickness may be
controlled by manipulation of relative TEOS and DMDES concentrations, or by quenching
the shell maturation step.
The second system involves the encapsulation of acidic or basic water-in-hexadecane
emulsions. These are prepared and exposed to small quantities of TEOS, thereby forming
a thin silica membrane at the water/oil interface. This skin was observed to crenellate, with
an optical microscope, upon evaporation of the aqueous core. Similar particles were also
prepared from emulsions initially stabilized with hydrophobic fumed silica. Thicker membranes
may be prepared if the aqueous phase also contains alkoxysilane monomer; these
skins survive washing with heptane, or centrifugation into water, and may be viewed by
SEM.
The coated PDMS particles were subjected to compression using a micromanipulator.
The capsule breaking force was found to be proportional to the shell thickness, as quantified
using SEM and ultramicrotomy. Model actives, such as dyes, may be incorporated into the
PDMS templates prior to shell formation through use of a vector solvent that swells the core
material.
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