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Preparation and investigation of Group 13 metal organo-phosphate hybrid -framework materials

Posted on:2010-07-07Degree:Ph.DType:Thesis
University:Wake Forest UniversityCandidate:Zhao, YueFull Text:PDF
GTID:2441390002985050Subject:Chemistry
Abstract/Summary:
Open-framework materials such as zeolites and low-dimensional materials such as metal phosphates have a wide range of applications in separation processes, catalysis, ion exchange, and intercalation chemistry. Current research in this field is focused on synthesizing hybrid inorganic-organic compounds, which combine inorganic species as nodes and organic species as linkers. These materials have been demonstrated to have versatile structures and show promising properties for applications in the areas of separation, catalysis, magnetism, photo-physics, and electronics.;The controlled synthesis of these materials is an ongoing challenge that offers tremendous opportunities in the area of materials science. The objective of the research conducted within the framework of this dissertation is to prepare and characterize hybrid framework metal organo-phosphate materials (MOPs). The idea is to use specific building units that can be linked or modified by functional organic groups to make materials with specific architectures and thus specific properties. The objective is to reach an understanding of how the organic and inorganic pieces fit together to allow for the preparation of tailor-made materials with specific structures and specific functionality of this type of materials.;The synthetic method of choice is a mild hydro- or solvo-thermal method in which the reactants and solvent are sealed in a container and heated slightly above the boiling point of the solvent under autogeneous pressure. Their structural characterization was done by single crystal X-ray diffraction. The presence of the organic moieties was determined by the combination of elemental analysis, XRD and IR spectroscopy. The thermal stability of these materials was determined by a combination of thermogravimetric analysis, IR spectroscopy, and powder XRD.;The study has led to the preparation and complete characterization of a number of new MOP materials with novel structures. They show a great diversity of structural topologies, coordination types, dimensionalities, pore sizes and physical or chemical properties. The MOPs synthesized and characterized can be classified in three different types of hybrid frameworks: (1) Hybrid frameworks built of pure inorganic metal phosphates (MPO4) layer or chains linked or coordinated by multitopic organic ligands such as oxalate, 1,10-phenanthroline and 4,4'-bipyridine. (2) Hybrid frameworks built of metal phosphonates (MPO3R) or metal diphosphonates (MPO 3RPO3). In this case the organic functional group is embedded in the inorganic framework. (3) Hybrid frameworks that can be considered to be a combination of the previous two types. They are built of metal phosphonate (MPO3R) layers or chains linked or coordinated by multitopic organic ligands.
Keywords/Search Tags:Metal, Materials, Hybrid, Framework, Organic, Preparation
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