Ke. Hamilton et al., THE ROLE OF REACTANT TRANSPORT IN DETERMINING THE PROPERTIES OF NIF SHELLS MADE BY INTERFACIAL POLYCONDENSATION, Fusion technology, 31(4), 1997, pp. 391-401
Polymer shells up to 2 mm in diameter were prepared using an interfaci
al polycondensation/cross-linking reaction occurring at the surface of
an oil drop. The oil phase is comprised of a solution (20 wt% or less
) of isophthaloyl dichloride (IPC) dissolved in an organic solvent. An
interfacial reaction is initiated when the IPC-loaded oil drop is sub
merged in an aqueous solution of poly(p-vinylphenol) (PVP), a poly(ele
ctrolyte) at elevated pH. Composition, structure, and surface finish f
or fully-formed dry shells were assessed using a number of techniques
including scanning electron microscopy (SEM), atomic force microscopy
(AFM), fourier-transform infrared spectroscopy (FTIR), pyrolysis-gas c
hromatography (GC)-mass spectroscopy (MS), microhardness measurements,
gas permeability, and solvent permeability measurements. From deposit
ion rate data, a reaction mechanism and key reaction parameters were i
dentified. The deposition rate of shell membrane material was found to
be a diffusion limited reaction of IPC through the forming membrane t
o the exterior shell interface (which is believed to be the reaction f
ront). The final thickness of the film deposited at the interface and
the rate of deposition were found to be strong functions of the IPC co
ncentration and oil phase solvent. Films made with diethyl phthalate (
DEP) were thinner and harder than films made using 1,6-dichlorohexane
(DCH) as a solvent. Differences in solubility of the forming membrane
in DCH and DEP appear to be able to account for the differences in dep
osition rate and the hardness (related to cross-linking density). The
deposition can be thought of as a phase separation which is affected b
y both the poly(electrolyte)/ionomer transition and the amount of cros
s-linking. Finally, it was found that the choice of oil phase solvent
profoundly affects the evolution of the outer surface roughness.