Growth and characterization of centimeter-sized crystals of pyridine dodecasil-3C
Marquart, Todd A.
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https://hdl.handle.net/2142/19378
Description
Title
Growth and characterization of centimeter-sized crystals of pyridine dodecasil-3C
Author(s)
Marquart, Todd A.
Issue Date
1994
Doctoral Committee Chair(s)
Klemperer, Walter G.
Department of Study
Chemistry
Discipline
Chemistry
Degree Granting Institution
University of Illinois at Urbana-Champaign
Degree Name
Ph.D.
Degree Level
Dissertation
Keyword(s)
Chemistry, Inorganic
Language
eng
Abstract
Hydrothermal seeded growth was used to grow centimeter-sized crystals of the all-silica zeolite ZSM-39, also known as the clathrasil dodecasil-3C (D3C). Through careful optimization of reaction conditions coupled with judicious choice of silica sources, conditions were found that minimize the effects of Ostwald's rule of successive transformations allowing for the growth of large, high-purity crystals of the metastable zeolite. The twinning present in pyridine D3C crystals was removed by thermal methods. X-ray single crystal studies of detwinned crystals coupled with data from optical crystallography studies were used to determine the structure at ambient temperature. The high-temperature structure was also determined by single crystal X-ray diffraction methods carried out at temperatures above the phase transformation at 161$\sp\circ$C. Twinning in both the ambient and high-temperature phases was examined. In order to examine the position and motion of the guest molecule, a combination of computer simulations and $\sp2$H NMR studies was undertaken.
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