We investigate the development of mesophase order in
compositionally asymmetric (13 wt
% styrene) polystyrene−polyisoprene (SI) diblock and SIS triblock
copolymers. The equilibrium ordered
morphology of these polymers is a body-centered-cubic (bcc) lattice of
spherical S microdomains. The
ordering kinetics are measured by quenching the material from above the
order−disorder transition
temperature (T
ODT) to a temperature where the
ordered phase is stable and following the structure
development by time-resolved small-angle X-ray scattering and dynamic
oscillatory rheological measurements. The kinetics are significantly slower than those observed
for nearly symmetric polymers of similar
T
ODT, resulting in a wider range of
experimentally accessible quench depths. The temporal evolution
of
the storage modulus G‘ measured at constant frequency
displays a two-step increase after a quench from
above the ODT, for sufficiently low temperatures and/or high molecular
weights. The long-time step
corresponds to the development of a bcc lattice of spherical
microdomains, while the first step results
from the finite time required for large-amplitude composition
fluctuations to develop fully.
Quality sample preparation for SEM is important to observe fine details without artifacts, and good preparation requires proper fixation, dehydration, drying and coating, An alternative 5 min passage in hexamethyldisilazane (HMDS) can replace critical point crying (CPD) and gives satisfactory results on many biological samples. CPD procedure may take up to 1 h per sample to ensure adequate drying, therefore a brief rinse in HMDS followed by air drying requires less time and equipment yet provides excellent results.Various biological samples were fixed in 3% glutaraldehyde; rinsed 3 times in Millonig's phosphate buffer for 10 min each; post-fixed in 1% osmium tetroxide for 1 h; rinsed as before; fixed again in 1% tannic acid (TA) for 30 min-1 h; rinsed well and partially dehydrated to 70% ethanol; placed in 1% uranyl-acetate (UA) in the dark, overnight: rinsed with 70% ethanol until UA cleared and then dehydrated through 100% ethanol.
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