The preparation of macro-micro bifunctional porous materials has been accom
plished by a well-controlled, vacuum-assisted technique. Monodisperse polys
tyrene latex spheres were ordered into close-packed arrays by slow sediment
ation, allowing a high flux of water through the interstices between latex
spheres. Zeolite LTA, FAU, LTL, BEA, MFI and Si-MFI nanocrystals, synthesiz
ed by hydrothermal procedures, permeated the interstices of latex spheres u
nder the driving force of flowing water. After drying and calcination at 50
0 degreesC, both the latex spheres and zeolite structure-directing molecule
s were removed, followed by the formation of products consisting of both cr
ystalline micropores and periodic, interconnected networks of submicron mac
ropores. XRD, SEM, TEM, IR, TG/DTA, ICP and N-2 adsorption-desorption measu
rements were performed to monitor the preparation and to characterize the p
roperties of the macro-micro bifunctional porous materials. The materials p
resented in this paper combine the benefits of both the micropore and macro
pore regimes. They could potentially improve the efficiency of both separat
ion and catalysis of zeolites.