TY - JOUR
T1 - Small angle X-ray scattering from MCM-41 and its synthesis gels
T2 - optimisation of the synthesis parameters
AU - Edler, K. J.
AU - Dougherty, J.
AU - Durand, R.
AU - Iton, L.
AU - Kirton, G.
AU - Lockhart, G.
AU - Wang, Z.
AU - Withers, R.
AU - White, J. W.
PY - 1995/9/13
Y1 - 1995/9/13
N2 - We have found optimised conditions for alkaline synthesis of the large pore molecular sieve, MCM-41, by determining small angle X-ray scattering and adsorption isotherms from materials at various stages of the preparation. The presence of highly curved surfaces, sealed structures, and quasicrystalline hexagonal products coexisting with true MCM-41 are all detected by transmission electron microscopy. Calcination must be carried out with care. The product is most crystalline from unstirred preparations which have been heated at 100°C for no longer than three days. Under these conditions, a maximum BET surface area of 1950 m2 g-1 was attained, with evident crystallinity observed by electron diffraction and transmission electron microscopy. In the stirred system, which appears to be in a non-equilibrium state, materials after calcination exhibiting Bragg d-spacings of 35 Å, 37 Å and 38 Å have been identified.
AB - We have found optimised conditions for alkaline synthesis of the large pore molecular sieve, MCM-41, by determining small angle X-ray scattering and adsorption isotherms from materials at various stages of the preparation. The presence of highly curved surfaces, sealed structures, and quasicrystalline hexagonal products coexisting with true MCM-41 are all detected by transmission electron microscopy. Calcination must be carried out with care. The product is most crystalline from unstirred preparations which have been heated at 100°C for no longer than three days. Under these conditions, a maximum BET surface area of 1950 m2 g-1 was attained, with evident crystallinity observed by electron diffraction and transmission electron microscopy. In the stirred system, which appears to be in a non-equilibrium state, materials after calcination exhibiting Bragg d-spacings of 35 Å, 37 Å and 38 Å have been identified.
KW - Characterisation
KW - Mesoporous molecular sieve
KW - Synthesis
U2 - 10.1016/0927-7757(95)03241-5
DO - 10.1016/0927-7757(95)03241-5
M3 - Article
AN - SCOPUS:0002256775
SN - 0927-7757
VL - 102
SP - 213
EP - 230
JO - Colloids and Surfaces A: Physicochemical and Engineering Aspects
JF - Colloids and Surfaces A: Physicochemical and Engineering Aspects
IS - C
ER -