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About this book

This book focuses on structural characterisation techniques for porous materials. Covering a range of techniques, including gas sorption, mercury porosimetry, thermoporometry, NMR and imaging methods, this practical guide presents the basic theory behind each characterisation technique, and discusses the practicalities of the experimental and data analysis approaches needed for complex industrial samples.

The book shows readers how to approach characterising a particular sort of material for the first time and then how to develop a strategy for more in-depth analysis. It also demonstrates how to determine the best techniques for solving particular problems, and describes methods of obtaining the required information, as well as the limitations of various methods. It particularly highlights a scientific approach involving parameter validation and simple acquisition.

Featuring examples taken from case studies of real-world industrial materials, this book is intended for industrial practitioners and researchers. It provides a manual of potential techniques and answers questions concerning porous materials that arise in areas such as the catalyst industry, the oil and gas sector, batteries, fuel cells, tissue engineering scaffolds and drug delivery devices.

Table of Contents

Frontmatter

Chapter 1. Introduction

Abstract
The basic aim of this book is to give an introduction to the many and varied ways of characterising porous solids. It assumes a basic knowledge of geometry, and basic chemistry and physics of the level of a typical undergraduate in the sciences or engineering.
Sean Patrick Rigby

Chapter 2. Gas Sorption

Abstract
This chapter first reviews the basic theory underlying adsorption-based methods. It then highlights some key issues, beyond what is normally found in apparatus manuals, which arise when conducting experiments. The particular reasons for the choice of adsorbate to characterise a given adsorbent are then discussed. The types of data that can be obtained from various types of sorption experiments are then described, along with suggestions for several different data analysis methods to deliver a range of descriptors for porous solids. These include surface area, pore sizes, surface roughness, pore connectivity, pore length, and degree of spatial heterogeneity.
Sean Patrick Rigby

Chapter 3. Mercury Porosimetry

Abstract
This chapter first explains the basic underlying theory for the mercury porosimetry technique. It then discusses some experimental issues not normally covered in any length in manuals for commercially available apparatus, particularly how data analysis changes depending upon the mechanical properties of the sample studied. The next section then describes the range of different sorts of experiments that can be performed with a commercial porosimeter, how the data can be analysed, and the types of void space descriptors that can be obtained. It will be seen that mercury porosimetry can provide information on more than just exterior pore neck size distributions but also surface area, pore network connectivity and degree of spatial heterogeneity. It will also be shown how porosimetry can be made an absolute rather than a relative measure of pore sizes.
Sean Patrick Rigby

Chapter 4. Thermoporometry and Scattering

Abstract
This chapter describes two techniques which generally share the attributes of often needing only minimal sample preparation and/or no additional probe fluid. It covers the basic underlying theory and experimental considerations for both thermoporometry and scattering methods. It discusses the idiosyncratic physical effects associated with, and the particular capabilities of, each type of method, and how these may deliver a range of different descriptors when a suitable experimental method is chosen, and the correct data analysis is employed. It will be shown how descriptors for surface areas, pore and particle size distributions, pore connectivity and pore size spatial correlations can be obtained.
Sean Patrick Rigby

Chapter 5. Nuclear Magnetic Resonance and Microscopy Methods

Abstract
This chapter describes the underlying theory of NMR and its various techniques suitable for porous media, including magnetic resonance imaging (MRI). It also includes the theory for complementary imaging methods, including computerised X-ray tomography (CXT), and several electron, and dual-beam microscopy methods. It discusses special considerations for sample preparation and experimental design, and the origins of potential image artefacts. The chapter describes a number of different NMR methods, which can be often coupled with MRI to additionally make spatially resolved, that can deliver combined structure and transport information on the same sample with the same probe fluid. The chapter will also discuss the complementary capabilities of the various other imaging modalities.
Sean Patrick Rigby

Chapter 6. Hybrid Methods

Abstract
This chapter first discusses the strategic rationale for the creation of hybrid characterisation methods, especially how idiosyncratic deleterious or useful characteristics of different techniques can be overcome or enhanced, respectively, by fully integrated combination with other different methods. It also describes how such hybrid methods are essential to ensure that the emergent pore–pore co-operative effects seen for networks are not a confuscating problem for data analysis but, actually, are a potential tool to obtain more information on more complex disordered network structures. The chapter then describes a number of different combinations of the techniques discussed in earlier chapters, including how the experiments can be integrated and the particular data analysis needed for the resulting combined data sets.
Sean Patrick Rigby

Chapter 7. Structural Characterisation in Adsorbent and Catalyst Design

Abstract
This chapter discusses the special experimental and data analysis considerations that relate to characterising industrial products, especially the key aims of characterising these materials, such as relating fabrication method to product performance. It will look at the particular questions that pore characterisation data is most often used to try to answer about industrial materials, such as the relationship between structure and activity in catalysts.
Sean Patrick Rigby

Chapter 8. Pore Structural Characterisation in Engineering Geology

Abstract
This chapter will consider the particular issues that arise in the pore characterisation of natural materials, especially rocks. It will briefly describe the origins of pores in rock materials and consider pore classification schemes as they relate to rocks. The chapter will discuss particular experimental considerations that especially arise for rocks, such as sampling and sample preparation. It will then describe how characterisation methods can be used to answer some of the key questions that arise for rocks, such as how to determine permeability, or hydrocarbon producibility, measures. It will also discuss particular data-handling and analysis issues that arise for rocks. This chapter will further describe special experimental techniques for studying materials with multi-scale heterogeneity, such as multi-modal imaging methods, gas overcondensation, and phenomenological ‘filtering’.
Sean Patrick Rigby
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