U. Costantino et F. Marmottini, INTERCALATION OF INSULATING POLYMERS INTO LAYERED ZIRCONIUM-PHOSPHATES, Materials chemistry and physics, 35(3-4), 1993, pp. 193-198
The ability of layered alpha- and gamma-zirconium phosphates to interc
alate directly some insulating oligomers (PEG 300 Da, PEG 600 Da) or p
olymers (PEO 2 x 10(5) Da, PEO 6 x 10(5) Da, PEI 2 x 10(5) Da) has bee
n investigated. The intercalation was obtained by various synthetic st
rategies: the zirconium phosphates, pre-swelled with ethanol or butano
l, were equilibrated with the oligomers as such or with the polymers d
issolved in organic solvents at different temperatures; PEO of various
molecular weights was intercalated by bringing the hosts into contact
with the polymers held at a temperature a little higher than that of
their glass transition. Intercalation compounds of alpha-zirconium pho
sphate with PEG 300 and PEG 600 have also been obtained by leaving the
host to form in the presence of the oligomers. The composites thus ob
tained have been characterized by H, C, N elemental analysis, XRD powd
er patterns at room and high temperature and TG-DTA coupled analysis.
The composition of the intercalates, expressed as moles of monomer per
mole of Zr, ranges from 1 to 2.2. The observed expansion of the inter
layer distance suggests that the polymers are intercalated with the ch
ain axis parallel to the layer plane; in only one case does the expans
ion indicate the presence in the interlayer region of the polymer in a
coiled conformation. The PEG and PEO guests are displaced when the co
mposites are washed with water or exposed to NH3 vapor or heated at te
mperatures higher than 180-degrees-C.