X-ray scattering and electron microscopy were used to characterize the structure of poly(ethylene-
alt-propylene-
block-ethylene oxide-
block-n-hexyl methacrylate) (PEP-
b-PEO-
b-PHMA) triblock copolymer/aluminosilicate hybrid materials in which the volume fraction of the PEP end-block (0.09 ≤
fPEP ≤ 0.12) was much smaller than that of the PEO-aluminosilicate (0.28 ≤
fPEO+aluminosilicate ≤ 0.44) and PHMA (0.47 ≤
fPHMA ≤ 0.60) domains. These hybrid compounds formed a hexagonally
patterned lamellar morphology in which the lamellae were aligned parallel to the material surface (lamellar repeat spacing = 33.0
![](http://pubs.acs.org/images/entities/plusmn.gif)
3.3 nm, in-plane row spacing = 21.7
![](http://pubs.acs.org/images/entities/plusmn.gif)
1.9 nm). Both the PHMA and PEO-aluminosilicate phases formed continuous, two-dimensional domains permitting individual sheets of the material to be isolated by
dispersal in organic solvent. Within each sheet, the lamellar PEO-aluminosilicate domain was hexagonally
patterned by an array of “holes” with lower aluminosilicate density. Since the enthalpy of mixing for the small PEP end-block and PEO-aluminosilicate phase is very large, the “holes” in the PEO-aluminosilicate sheet may correspond to micellar PEP domains forming either dimples in the surface of the sheet or pillars spanning the sheet as in the proposed “pillared-lamellae” morphology (
Macromolecules 2001,
34, 6994−7008). These results suggest that the use of ABC copolymers as structure-directing agents may provide access to a wide range of morphologies.