TY - BOOK AU - Aligizaki,Kalliopi K. TI - Pore structure of cement-based materials: testing, interpretation and requirements T2 - Modern concrete technology series SN - 0419228004 AV - TA435 .A48 2006 PY - 2006/// CY - Abingdon [England], New York PB - Taylor and Francis KW - Cement KW - Testing KW - Porosity N1 - 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 ER -