Pore structure of cement-based materials : testing, interpretation and requirements / Kalliopi K. Aligizaki.

Includes bibliographical references and index.

Preface Acknowledgements Conversions Symbols Abbreviations List of figures List of tables Chapter 1 INTRODUCTION 1.1 SCOPE OF THE BOOK 1.2 PORES IN CEMENT PASTE 1.2.1 Gel pores 1.2.2 Capillary pores 1.2.3 Hollow-shell pores 1.2.4 Air voids 1.2.5 Pore size ranges 1.3 METHODS FOR CHARACTERIZING PORE STRUCTURE 1.4 DEFINITION OF PORE STRUCTURE PARAMETERS 1.4.1 General pores 1.4.1.1 Porosity 1.4.1.2 Hydraulic radius 1.4.1.3 Specific surface area 1.4.1.4 Threshold diameter 1.4.1.5 Pore size distribution 1.4.1.6 Other parameters 1.4.1.7 Factors affecting the parameters measured 1.4.2. Air voids 1.4.2.1. Total air content 1.4.2.2 Specific surface 1.4.2.3 Spacing factor References Chapter 2 SPECIMEN PRETREATMENT 2.1 WATER REMOVAL 2.1.1 Drying techniques 2.1.1.1 Oven-drying 2.1.1.2 Vacuum-drying 2.1.1.3 P-drying 2.1.1.4 D-drying 2.1.1.5 Direct freeze-drying 2.1.1.6 Indirect freeze-drying 2.1.1.7 Desiccant drying 2.1.1.8 Critical Point Drying 2.1.2 Solvent Replacement 2.1.2.1 Ease of penetration 2.1.2.2 Physical and chemical interactions 2.1.3 Comparison of different water removal techniques 2.2 PREPARATION FOR MICROSCOPY 2.2.1 Polished surface 2.2.1.1 Cutting, grinding and polishing 2.2.1.2 Impregnation by epoxy resin · Dry vacuum impregnation · Fluorescent liquid replacement 2.2.2 Thin sections 2.2.3 Fractured surface 2.2.4 Intrusion alloys References Chapter 3 MERCURY INTRUSION POROSIMETRY 3.1 THEORY AND TESTING PROCEDURE 3.1.1 Instrument description 3.1.2 Testing procedure 3.1.2.1 Low pressure 3.1.2.2 High pressure 3.1.3 Calculation of pore size 3.1.4 Pore size distribution 3.1.5 Specific surface area 3.2 PLOTS OBTAINED 3.2.1 Cumulative intrusion curve 3.2.2 Incremental and differential distribution curve 3.2.3 Surface area 3.2.4 Range of sizes determined 3.3 HYSTERESIS AND ENTRAPMENT OF MERCURY 3.3.1 Theories proposed to explain hysteresis 3.3.1.1 Ink-bottle pores and trapped mercury 3.3.1.2 Contact angle hysteresis 3.3.1.3 Pore potential theory 3.3.1.4 Surface roughness 3.3.1.5 Compression of the solid 3.3.2 Entrapment of mercury and second intrusion method 3.4 PARAMETERS AFFECTING RESULTS 3.4.1 Specimen pretreatment 3.4.2 Specimen size 3.4.3 Rate of pressure build-up 3.4.4 Contact angle 3.4.4.1 Parameters affecting contact angle Cement paste characteristics Pore size Mercury purity Surface roughness 3.4.4.2 Determination of contact angle 3.4.5 Surface tension of mercury 3.4.6 Alteration of pore structure 3.4.7 Alternative intrusion liquids 3.5 ADVANTAGES AND LIMITATIONS References Chapter 4 GAS ADSORPTION 4.1 THEORY AND TESTING PROCEDURE 4.2 ANALYSIS OF DATA 4.2.1 Adsorption isotherm 4.2.2 Thickness of adsorbed film 4.2.3 Pore size (Kelvin Equation) 4.3 TOTAL PORE VOLUME 4.3.1 Dubinin-Radushkevich equation 4.4 PORE SIZE DISTRIBUTION 4.4.1 The Barrett-Joyner-Halenda method 4.4.2 The Cranston-Inkley method 4.4.3 The Modelless method and Micropore (MP) analysis method a) Modelless method [4.33] b) Micropore analysis method 4.5 SPECIFIC SURFACE 4.5.1 The Langmuir theory 4.5.2 The Brunauer-Emmett-Teller (BET) theory 4.5.3 The Dubinin-Kaganer equation 4.5.4 The Harkins-Jura (HJ) relative method 4.5.5 The t-plot 4.5.6?The ?s-plot 4.6 ADSORPTION HYSTERESIS 4.7 FACTORS AFFECTING THE RESULTS 4.7.1 Pretreatment method 4.7.2 Type of adsorbate used 4.7.3 Analysis method used 4.8 ADVANTAGES AND LIMITATIONS References Chapter 5 PYCNOMETRY AND THERMOPOROMETRY 5.1 PYCNOMETRY 5.1.1 Liquid pycnometry 5.1.1.1 Water absorption 5.1.1.2 Water replacement using an alcohol 5.1.2 Gas (Helium) Pycnometry and Helium Flow 5.1.2.1 Theoretical aspects 5.1.2.2 Helium flow 5.1.2.3Determination of surface area and hydraulic radius 5.1.2.4 Effect of pretreatment 5.1.3 Advantages and limiations 5.2 THERMOPOROMETRY 5.2.1 Theoretical considerations 5.2.2 Experimental procedure 5.2.3 Pore size distribution 5.2.4 Determination of the Surface Area and the Average Radius 5.2.5 Applications on cement paste 5.2.6 Advantages and limitations References Chapter 6 NUCLEAR MAGNETIC RESONANCE 6.1 THEORETICAL ASPECTS / FUNDAMENTALS 6.1.1 Single nucleus properties 6.1.2 Magnetization of a group of nuclei (bulk magnetization) Interactions between nuclei 6.2 NMR EXPERIMENT 6.2.1 Instrumentation 6.2.2 NMR excitation and response 6.2.2.1 Free Induction Decay 6.2.2.2 Fourier transformation and spectrum 6.2.3 Pulse sequences 6.2.3.1 Hahn spin echo pulse sequence 6.2.3.2 Inversion recovery pulse sequence 6.2.3.3 Carr-Purcell echo pulse sequence 6.3 SPIN RELAXATION 6.3.1 Spin-lattice relaxation 6.3.2 Spin-spin relaxation 6.3.3 Inhomogeneous broadening 6.4. PORE SIZE DETERMINATION 6.4.1 Magnetic Resonance Relaxation Analysis 6.4.1.1 Relaxation inside a single pore 6.4.1.2 Relaxation inside a distribution of pore sizes Discrete model Diffusion cell model 6.4.1.3 Pore size distribution in cement pastes 6.4.2 NMR Cryoporometry 6.4.3 NMR imaging 6.4.3.1 Strong field gradients 6.4.3.2 Fast Imaging methods 6.5.3.3 Application to porous materials 6.5 ADVANTAGES AND LIMITATIONS References Chapter 7 SMALL ANGLE SCATTERING 7.1 THEORETICAL ASPECTS 7.2 EXPERIMENTAL PROCEDURE 7.2.1 Small-angle X-ray scattering equipment setup 7.2.2 Small-angle neutron scattering equipment setup 7.2.3 Data collection/Measurement 7.3 PLOTS OBTAINED 7.3.1 Guinier's plot 7.3.2 Porod's plot 7.4 RANGE OF SIZES 7.5 APPLICATIONS TO CEMENT PASTES 7.5.1 Guinier plot 7.5.2 Porod plot 7.5.3 Scattering contrast 7.5.4 Surface area 7.5.5 Structure of cement paste 7.5.6 Fractal dimension 7.5.7 Factors affecting the results 7.5 ADVANTAGES AND LIMITATIONS References Chapter 8 MICROSCOPIC TECHNIQUES AND STEREOLOGY 8.1 OPTICAL MICROSCOPY 8.1.1 Types of Microscopes 8.1.2 Characteristics of the microscope 8.2 SCANNING ELECTRON MICROSCOPY 8.2.1 Design and physical basis of operation 8.2.2 The Performance and characteristics of the SEM 8.2.3 Electron-Specimen Interactions and principal images 8.2.3.1 Secondary electrons 8.2.3.2 Backscattered electrons (BSE) 8.2.4 Environmental (scanning) electron microscopy 8.2.5 Transmission electron microscope 8.3 SCANNING ACOUSTIC MICROSCOPY 8.4 IMAGE ANALYSIS 8.4.1 Image analysis steps 8.5 STEREOLOGY 8.5.1 Point Counting 8.5.2 Lineal Analysis 8.5.2.1 Pore volume 8.5.2.2 Pore size distribution 8.5.3 Section Analysis 8.5.3.1 Pore volume 8.5.3.2 Pore size distribution from section diameters 8.5.3.3 Pore size distribution from section areas 8.5.4 Comparison of stereological methods 8.5.4.1 Comparison for pore volume 8.5.4.2 Comparison for pore size distribution 8.6 APPLICATION OF MICROSCOPIC TECHNIQUES TO CEMENT PASTE MICROSTRUCTURE ANALYSIS 8.7 AIR VOIDS ANALYSIS USING OPTICAL MICROSCOPY 8.7.1 Factors affecting results 8.7.2 Different mathematical parameters 8.7.3 Image analysis of air voids 8.7.4 Section analysis used for air volume 8.7.5 Air void distribution References Chapter 9 COMPARISON OF RESULTS BY VARIOUS METHODS (Not final) 9.1 COMPARISON WITH MIP RESULTS 9.1.1 Nitrogen Adsorption Effect of pretreatment Reasons of differences 9.1.2 Helium pycnometry 9.1.3 Alcohol Exchange Water 9.1.4 NMR vs. MIP and Nitrogen Sorption 9.1.5. Small Angle X-Ray Scattering 9.2 COMPARISON WITH NITROGEN ADSORPTION 9.2.1 Helium Pycnometry 9.2.2 Water Sorption 9.2.3 SAXS Vs. Nitrogen Adsorption And Drying 9.3 COMPARISON WITH REPLACEMENT TECHNIQUES 9.3.1 Helium Pycnometry Vs. Methanol Sorption 9.3.2 Alcohol Exchange Vs. Water Saturation 9.3.3 Evaporable Water Vs. Rewetting 9.3.4 Neutron scattering vs. water evaporation 9.3.5 SAXS vs. water sorption 9.4 COMPARISON WITH MICROSCOPY TECHNIQUES Image analysis using BSE 9.1.6 MIP vs. SEM MIP vs OM MIP vs. image analysis by SEM Pore size distribution Image analysis vs.

methanol adsorption References CONCLUSIONS Standards Glossary of terms Index of terms Author index