cm035283j_si_001.pdf (108.41 kB)
Self-Assembly of Colloidal Zeolite Precursors into Extended Hierarchically Ordered Solids
journal contribution
posted on 2004-08-10, 00:00 authored by C. Shane Carr, Stefan Kaskel, Daniel F. ShantzA new porous material containing both micropores and mesopores has been synthesized
by the self-assembly of silicalite-1 colloidal precursors at low temperatures and thoroughly
investigated by diffraction, electron microscopy, porosimetry, and spectroscopy. Our “bottom-up” approach yields mesoporous materials that contain a microporosity different from that
of SBA-15. For the samples where the silicalite-1 mixture is aged at room temperature, we
do not have conclusive evidence that silicalite-1 is responsible for the microporosity in our
samples, as all analytical techniques are inconclusive. By contrast, samples where the
silicalite-1 mixture is heated until Bragg reflections are observed appear by TEM to be
heterogeneous materials containing both mesopores and domains of silicalite-1. Nitrogen
and argon adsorption show that both the micropore size distribution and the total micropore
volume of our samples are different from those of SBA-15. The conclusions from this study
are fourfold: (1) we have created a material containing both micropores and mesopores that
is very well ordered on the mesoscale, (2) our material has a larger micropore volume and
different micropore size distribution than SBA-15 made under the same conditions, (3) we
have achieved this high degree of structural ordering and uniformity without the need for
high-temperature syntheses, and (4) it does not appear possible to use larger (∼50 nm)
nanoparticles of silicalite-1 to fabricate homogeneous materials. The ability to synthesize
these materials at low temperatures makes them (and the synthetic concept) ideal for
extension into areas such as thin-film syntheses.