R. Singh et Pk. Dutta, Crystal growth of faujasitic microporous zincophosphate crystals using reverse micelles as reactants, LANGMUIR, 16(9), 2000, pp. 4148-4153
The present study deals with the crystallization of zincophosphate-X (ZnPO-
X) from zinc- and phosphate-containing reverse micelles. ZnPO-X has the sam
e topology as faujasite (zeolites X,Y). Reverse micelles are microdroplets
of water stabilized in a hydrocarbon medium with the help of surfactants. S
uccessful synthesis of ZnPO-X was possible using reverse micelles made with
cationic surfactant dimethyldioctylammonium chloride (DODMAC), l-decanol a
s cosurfactant and isooctane as solvent, The composition of the reactants i
n the water pools of the reverse micelles was about four times more dilute
than that in a conventional hydrothermal synthesis. The dilution is necessa
ry since a significant fraction of the water in the reverse micelles is use
d up for hydrating the headgroups of the surfactant. The crystals appear wi
thout the formation of an intermediate amorphous phase. Upon mixing the zin
c and phosphate reverse micelles, collisions between them result in exchang
e of reactants. We propose that only a small fraction of these reverse mice
lles have the proper supersaturation conditions for nucleation of ZnPO-X. T
hese nuclei then grow into crystals by incorporating nutrients from non-nuc
leated reverse micelles. In a typical synthesis, only about 15-20% of the p
ossible yield of ZnPO-X was obtained and the rest of the material remained
suspended in the organic phase. This clear suspension was an excellent seed
solution for ZnPO-X, even from reverse micelle compositions that would not
produce ZnPO-X. Using this seed solution and reaction columns of different
lengths, crystals of different sizes could be obtained. Reverse micelles a
s reactants appear to provide a novel way to control supersaturation and th
ereby influence crystal growth of microporous structures in ways that canno
t be readily done with conventional procedures of synthesis of these import
ant materials.