This cumulative dissertation is a compendium of five peer-reviewed and published
scientific papers on developing an advanced NMR Cryoporometry toolbox for pore architecture characterization. The dissertation contains five chapters. The first introduces porous materials, their types and applications. Chapter two describes the fundamentals of fluid phase equilibria in mesoporous solids and how modifications of the well-known Laplace equation describe various fluid phase equilibria. The basic principles of the Gas Sorption and NMR Cryoporometry techniques are discussed. In chapter three, different characterization techniques are amalgamated onto a common framework which can be used to compare fluid phase coexistence in porous materials of different pore sizes. Chapter four explains a completely new NMR Cryoporometry characterization methodology developed for cylindrical and spherical pore shapes. Chapter five concludes and crowns the present work by discussing the complementary benefits of the advanced technique in characterizing random porous materials and accounting for pore connectivity effects. All materials synthesized for the work in this dissertation have been obtained through collaborations with the groups of Profs. Dr. Michael Fröba and Simone Mascotto of the Hamburg University and Prof. Dr. Dirk Enke of the Leipzig University.:Table of Contents
Thesis Summary ........................................................................................................1
List of publications ......................................................................................................2
Acknowledgements ...................................................................................................4
CHAPTER 1:.............................................................................................................10
Introduction ..............................................................................................................10
CHAPTER 2:.............................................................................................................12
Fluid Phase Equilibria in Mesoporous Solids ..........................................................12
2.1 Gas Sorption................................................................................................... 13
2.1.1 Adsorption Isotherms................................................................................ 15
2.1.2 Adsorption Hysteresis............................................................................... 18
2.1.3 Scanning Behavior.................................................................................... 23
2.2 NMR Cryoporometry ....................................................................................... 25
2.2.1 Pore Size Distribution (PSD)....................................................................... 28
2.3 Serially-Connected Pore Model (SCPM)......................................................... 29
2.4 Problem Statement ......................................................................................... 30
CHAPTER 3:..............................................................................................................32
Analogy between Characterization Techniques ......................................................32
• Publication 3. On the Comparative Analysis of Different Phase Coexistences
in Mesoporous Materials
CHAPTER 4:.............................................................................................................42
An Advanced NMR Cryoporometry Approach.........................................................42
• Publication 4.1. Nuclear Magnetic Resonance Cryoporometry Study of
Solid−Liquid Equilibria in Interconnected Spherical Nanocages
• Publication 4.2. A novel approach for advanced thermoporometry
characterization of mesoporous solids: Transition kernels and the serially
connected pore model
CHAPTER 5:.............................................................................................................65
Characterizing Random Porous Materials................................................................65
• Publication 5.1. Comparative Gas Sorption and Cryoporometry Study of
Mesoporous Glass Structure: Application of the Serially Connected Pore Model
• Publication 5.2. Impact of Geometrical Disorder on Phase Equilibria of Fluids and Solids Confined in Mesoporous Materials
Appendix A:.............................................................................................................100
Porous Solid Characterization Techniques............................................................100
A.1: Mercury Intrusion Porosimetry (MIP) ........................................................... 100
A.1.1. Experimental Set-up.............................................................................. 101
A.2: Gas Sorption................................................................................................ 103
A.2.1. Experimental Set-Up ............................................................................. 103
A.2: NMR Cryoporometry.................................................................................... 106
A.2.2. Experimental Set-Up ............................................................................. 106
Appendix B:..............................................................................................................109
Supporting information ............................................................................................109
Appendix C:.............................................................................................................115
Author contributions ................................................................................................115
Bibliography ............................................................................................................117
| Identifer | oai:union.ndltd.org:DRESDEN/oai:qucosa:de:qucosa:81955 |
| Date | 03 November 2022 |
| Creators | Enninful, Henry Reynolds Nana Benyin |
| Contributors | Universität Leipzig |
| Source Sets | Hochschulschriftenserver (HSSS) der SLUB Dresden |
| Language | English, German |
| Detected Language | English |
| Type | info:eu-repo/semantics/acceptedVersion, doc-type:doctoralThesis, info:eu-repo/semantics/doctoralThesis, doc-type:Text |
| Rights | info:eu-repo/semantics/openAccess |
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