Testing and Evaluation of Advanced Building Materials Edited by Wu Yao Testing and Evaluation of Advanced Building Materials Selected, peer reviewed papers from the First National Academic Symposium on Testing and Evaluation of Building Materials (TEBM 2012), June 22-24, 2012, Shanghai, China Edited by Wu Yao Copyright 2013 Trans Tech Publications Ltd, Switzerland All rights reserved. No part of the contents of this publication may be reproduced or transmitted in any form or by any means without the written permission of the publisher. Trans Tech Publications Ltd Kreuzstrasse 10 CH-8635 Durnten-Zurich Switzerland http://www.ttp.net Volume 539 of Key Engineering Materials ISSN print 1013-9826 ISSN cd 1662-9809 ISSN web 1662-9795 Full text available online at http://www.scientific.net Distributed worldwide by and in the Americas by Trans Tech Publications Ltd Trans Tech Publications Inc. Kreuzstrasse 10 PO Box 699, May Street CH-8635 Durnten-Zurich Enfield, NH 03748 Switzerland USA Phone: +1 (603) 632-7377 Fax: +41 (44) 922 10 33 Fax: +1 (603) 632-5611 e-mail: [email protected] e-mail: [email protected] Preface The First National Academic Symposium on Testing and Evaluation of Building Materials (TEBM 2012) was held from June 22 to 24, 2012 in Tongji University, Shanghai, China. The main aim of this symposium is to provide a platform for academics, industrialists and students from various regions of China to exchange ideas and the state-of-the-art development in the field of building materials and testing techniques. This symposium is also intended to foster a network and future collaborations between materials scientists, testing technologists and instrument manufactories, and has been proved to be successful. In this symposium, all papers were received from electronic submission system, which were peer reviewed. Finally, 53 papers were accepted for publication. The contents of papers include the microscopic theoretical model of the building materials, the characterization of the compositions and structures, performance testing and evaluation. These papers largely reflect the researching hotspots and the latest advances in the testing and evaluation theory and technology of building materials in China. The efforts of the participants of all manuscripts are greatly appreciated. The help and advice of Prof. Jianghong Gong of Tsinghua University are gratefully acknowledged. Thanks are also extended to the Trans Tech Publications Ltd for their publishing proceedings of TEBM 2012 in the periodical “Key Engineering Materials”. Prof. Wu Yao Tongji University, China Chairman, First National Symposium on Testing and Evaluation of Building Materials June, 2012 Table of Contents Preface 29Si NMR Characterization of Silica Tetrahedron in the Silica Fume Simulate Hydration X.J. Wang, X.Y. Wang, H.F. Zhu and C. Qian 1 Investigation of Early Cement Paste with 1H Low-Field NMR Z.P. Sun, Q. Li, Y. Yu and P.Q. Yang 5 The Application of Freezing-Melting Hysteresis in Hardened White Cement Paste Z.P. Wang, T. Wang and L. Zhou 10 An Experimental Study of Water in Pore System of Hardened Cement Paste by Magnetic Resonance A.M. She, W. Yao and W.C. Yuan 14 Quantitative Characterization of Hydration of Cement Pastes by Rietveld Phase Analysis and Thermoanalysis Y.Q. Wei and W. Yao 19 Kinetic Study of Portland Cement Hydration with Ground Penetrating Radar W. Chen, P.L. Shen, J.X. Lu and W.R. Zhang 25 Study on the Hydration Kinetics of Portland Cement W. Wang, W. Yao and Y.Q. Wei 30 Relationship between Internal Relative Humidity and Autogenous Shrinkage of Cement Paste with Supplementary Cementitious Materials (SCM) Y. Li and Q.Q. Yan 35 A Testing Device for Humidity-Control Performance of Pervious Concrete J.L. Wu, X. Wu and X.F. Lv 40 An Evaluation of Shrinkage Model Based upon Microstructure of Blended Cement Pastes Y. Chen, W. Yao and D. Jin 44 Early-Age Free Shrinkage of Mortars with Different Dosages of EVA Redispersible Powder S.F. Liu and P.M. Wang 49 Shrinkage of Blended Cement Pastes with Mineral Additions Y. Chen, W. Yao and D. Jin 55 Relative Humidity of Blended Cement Pastes in Sealed during Hydration D. Jin, W. Yao and Y. Chen 60 Effect of Hollow Glass Microsphere on Performance of Foam Concrete Q. Wang, L.G. Qiu, Q. Yao, Z.Y. Ding and X.F. Yan 64 Effects of Rubber Powder and Fly Ash on Mechanical Properties of Recycled Mortars Y.F. Meng, Y.Q. Wei, D.Z. Wang and K. Gao 70 Micromechanical Properties of Calcium Silicate Hydrate W. Yao and L. He 75 Probing Nanostructure of Calcium Silicate Hydrate by AFM and Nanoindentation K. Liang, W. Yao, L.J. Chen and Q. Gao 80 Study on the Unhydrated Cement Grain/C-S-H Gel Interface in Cement Paste by Use of Nano-Scratch Technique Y. Mao, W. Yao and J. Xu 84 Temperature Sensitive Properties of Hybrid Carbon Nanotube/Carbon Fiber Cement- Based Materials J.J. Qin, W. Yao and J.Q. Zuo 89 Research on Optimizing the Electrical and Mechanical Properties of Carbon Fiber Reinforced Cement J. Xu and W. Yao 94 Mechanical Property of Hybrid Steel Fiber Reinforced Cement-Based Composites H.T. Tan, W. Yao, X.M. Song and S. Dong 99 Enhancing the Thermoelectric Properties in Carbon Fiber/Cement Composites by Using Steel Slag J.Q. Zuo, W. Yao and J.J. Qin 103 Seismic Behaviour of RC Columns Strengthened with Steel Bar/Wire Mesh Mortar Y.H. Sun, X.Y. Wu and G.J. Xiong 108 b Testing and Evaluation of Advanced Building Materials Carbonation Profile of Cement Paste and Concrete Established with Micro-Hardness Analysis W. Chen, X.X. Chen and S.Z. Zhang 115 Effect of Activated Water Treatment Sludge on Carbonation of Mortar Y. Chen 120 Effect of Fly Ash on Resistance to Sulfate Attack of Cement-Based Materials K.W. Liu, M. Deng and L.W. Mo 124 Study of Durability Analysis and Evaluation Model for Existing Concrete Structure in Coastal Areas H.Y. Yu and H. Zhang 130 The Effect of Fly Ash on TSA of Cementitous Material: Based on Three Years Results B.W. Liu, C.H. Yang, X.B. Xiang, L.W. Yu and J. Zhang 139 Study of Mechanical Force on Coal Gangue Reactivity C.S. Zhang, X.F. Liu, Q.S. Wu, Y.X. Deng and L. Li 145 The Effect of Electrochemical Chloride Extraction Combining Ultrasonic on Steel- Reinforced Mortars X.M. Xing and W. Yao 149 Tentative Study on Sonoelectrochemical Chloride Extraction from Mortar Y.Q. Chen, W. Yao and X.M. Xing 153 Analysis of Bond and Anchorage Performances of Helical and Twisted Reinforcement Material J.L. Zhang and C.L. Wang 158 Research on Modification of Steady State Migration Test for Cementitious Materials J.B. Yang, P. Zhang and L.P. Wu 166 Study on Hydration Degree of Portland Cement-Slag Complex Binders R.G. Liu and P.Y. Yan 172 Study on Pore Structure Characterization of Concrete at Different Ages by Thermoporometry Z.W. Jiang, Z.L. Deng and N. Zhang 178 Determining the Contact Angle of Hardened Cement Paste Using Thin Layer Wicking Method Q. Tian, H. Zhang, Y.J. Wang, F. Guo, T. Yao and J.P. Liu 184 Solubility Behavior of the Hydration Products in the Pore Solution of Hydrated Cement Pastes W. Yao and M.J. Wu 189 Effect of Metakaolin on the Physical Properties and Setting Time of High Performance Concrete B.M. Wang, H.N. Ma, M. Li and Y. Han 195 The Effect of Curing System on Mechanical Properties of Desulphurization Gypsum-Slag Composite Binder X.Q. Liu, J. Wang and H.G. Qin 200 The Influence of Curing Temperature on the Coordination of the Expansion and Strength of High Strength Expansive Concrete J.J. Feng, C.L. Zhou, Y. Sun and X.Q. Wang 205 Preparation of MgO- and CaO-Bearing Expansive Agent Used for Cement-Based Materials L.W. Mo, Y. Deng, A.Q. Lu and M. Deng 211 Study on Compatibility of Modified the Cement-Based Composite Biomass Materials by Agent J. Liu, C. Lin, W.H. Sun and X.M. Wang 215 The Brief Analysis of Photovoltaic Insulating Glass in the Process Service W.H. Li, C. Li, Y. Qiu and C.G. Wei 220 Phosphate Bonding: A New Method for Using Large Volume of Fly Ash Z. Ding, M. Zhang, B.Q. Dong, W. Liu and H. Lu 225 The Preparation and Pozzolanic Activity of Metakaolin Admixtures B.M. Wang, Y. Zhang and M. Li 230 Influence of Steel Slag on the Workability of Concrete J.W. Yang, Q. Wang, P.Y. Yan and B. Zhang 235 Study on the Influence Factors of the Dispersion of Carbon Nanotubes in Aqueous Solution X.Y. Liu, Y. Xu, L. Chen, X.R. Wang and M.K. Zhou 239 Key Engineering Materials Vol. 539 c Properties of Cement Mortars Mixed with SiO and CaCO Nanoparticles 2 3 D.Z. Wang, Y.Y. Zhang and Y.F. Meng 244 Alkali Activity of Granite Aggregates and Control in the Concrete of the Three Gorges Project Z.Q. Wang, C.X. Liu, Z.Y. Wen, Z. Li and L. Xiao 249 Preparation of AgBr Nanowire Arrays in Porous Anodic Aluminium Oxide Template by Paired Cell Deposition M.M. Cui, X.C. Yang and J.W. Hou 255 Influence and Mechanisms of In Situ Toughening Telechelic Polymer on the Microstructure of Concrete X.B. Zhu, P. Feng, J.P. Liu, B. Ding and J.X. Hong 259 Research on the Application of Liquid Permeating Method to Silica Sol Stability L. Li, N. Zhou, X. Cui and W.H. Huang 266 Environmentally Friendly Cellular Concrete for Wall Insulation Y.Q. Jiang, J. Yang and Y. Chen 271 Key Engineering Materials Vol. 539 (2013) pp 1-4 © (2013) Trans Tech Publications, Switzerland doi:10.4028/www.scientific.net/KEM.539.1 29Si NMR Characterization of Silica Tetrahedron in the Silica Fume Simulate Hydration Xiaojun Wang1, a, Xiaoyao Wang2, 3, Hongfei Zhu1 and Cheng Qian1 1College of Materials Science and Engineering, Nanjing University of Technology, Nanjing 210009, China 2Department of Building Engineering, Tongji University, Shanghai 200092, China 3Depatrment of Civil Engineering and Environmental Engineering, Virginia Tech., Blacksburg, VA 24061, USA a [email protected] Keywords: Silica fume; Silica tetrahedron; Hydration; Nuclear magnetic resonance Abstract. As the major structure of silica fume, the change of silica tetrahedron in the pozzolanic reaction during the hydration has not been revealed clearly in previous studies. In this study, 29Si solid-state MAS NMR was used to characterize the silica tetrahedron change of the silica fume in saturated alkali solution with 0.9, 1.2, 1.5 and 1.8 four different calcium/silica ratios. The amorphous Q4 silica tetrahedron structure in silica fume changed into Q1 silica tetrahedron at 1 day. Q2 silica tetrahedron formed from Q1 silica tetrahedron within 3 days. Q1 and Q2 silica tetrahedron reached a balance until silica fume completed pozzolanic reaction and the Q4 silica tetrahedron exhausted. The coexistence of Q1 and Q2 silica tetrahedron benefited the physical properties increase of cementitious system. 29Si solid-state MAS NMR results proved that the chain length of silica tetrahedron in C-S-H shortened in the silica fume hydration while the C/S ratio increased. Introduction Silica fume is widely used in blended cement or concrete as a fine and highly pozzolanic cement replacement blend. The mechanism and the influence of silica fume in cement and concrete are hot spots of research. The previous researches focused on the factors, such as water/binder ratio, hydration degree, setting time, consistency, shrinkage, compression strength and permeability of cement paste or concrete with silica fume [1-11]. Furthermore, the hydration model and hydration kinetics aroused the researchers’ attention as well [12-14]. In the aforementioned works, it was mentioned that silica fume could react with calcium hydroxide and constitute the hydrated calcium silicate (C-S-H), which diluted the alkali concentration, reduced the influence of alkali-aggregate reaction (AAR), and played an important role in the strength of the cement pasta or concrete. The pozzolanic reaction of silica fume was expressed as 3CH+2S→C S H [15], particularly, without the 3 2 3 silica tetrahedron characterization of silica fume in the hydration process. Brunet and Lv reported that the chain length of silica tetrahedron became shorten as the calcium/silica ratio increase [16,17]. There were few reports about the silica tetrahedron change in the system with various C/S ratios. As for the pozzolanic reaction of silica fume, the change of silica tetrahedron as the C-S-H forms still remains unclear. As a result, it is necessary to find the change of silica tetrahedron in silica fume pozzolanic reaction and to predict the silica fume effect on blended cement or concrete based on silica tetrahedron change. In this work, 29Si solid-state MAS NMR investigations on the silica tetrahedron change of the silica fume in saturated alkali solution were reported for four different calcium/silica ratios: 0.9, 1.2, 1.5 and 1.8, respectively. Specimen of silica fume in simulated hydration were detected during a period of 90 days from initial state, and compared with silica tetrahedron change. The information was gathered about the silica tetrahedron and the chain length of the silica tetrahedron in the C-S-H phase was determined. This study provides a reference for the silica tetrahedron research of blended cement or concrete with silica fume. 2 Testing and Evaluation of Advanced Building Materials Experimental Silica fume was manufactured by Elcon, with a surface area of 18,900 m2/kg measured by the BET nitrogen sorption method, and the chemical composition is listed in Table 1. Calcium hydroxide was from Lingfeng chemical Co. Ltd. in Shanghai containing more than 95.0% calcium hydroxide. According to four different C/S ratios of 0.9, 1.2, 1.5 and 1.8, silica fume was stirred incessantly in a tank with saturated calcium hydroxide solution filled (with pH=13 and certain calcium hydroxide), where the ambient temperature was kept at 293 K. The specimens were measured by 29Si solid-state MAS NMR in prescribed age. The samples were accurately weighed and then filled into an NMR sample tube. The 29Si solid-state nuclear magnetic resonance experiments were performed on a Bruker Avance 400 (9.39 T, 79.5 MHz) using a home built CP/MAS probe for 4mm zirconia rotors, a spinning speed of 8 kHz, single pulse excitation with a pulse width of 4 µs, and relaxation delay of 8 s and 10000 scans. Chemical shift refers to an external standard of tetramethylsilane at 0 ppm. Table 1 Chemical composition of silicon fume /wt% Materials Loss SO SiO Fe O Al O CaO MgO K O Na O 3 2 2 3 2 2 2 CSF 2.57 1.00 91.36 0.28 0.63 0.63 1.96 1.19 0.52 90d 90d 56d 56d 28d 28d 14d 14d 7d 7d 3d 3d 1d 1d -60 -70 -80 -90 -100-110-120-130-140 -60 -70 -80 -90 -100 -110 -120 -130 -140 δδδδ Si / ∗∗∗∗ 10-6 δδδδ Si / ∗∗∗∗ 10-6 (a) (b) Figure 1 29Si NMR spectra of silica fume with the C/S ratios of (a) 0.9 C/S and (b) 1.8 C/S Figure 2 The silica tetrahedron structural changes of silica fume in simulate hydration Results and Discussion 29Si solid-state NMR of silica tetrahedron in the silica fume simulate hydration. The 29Si solid- state NMR spectra of silica tetrahedron in the silica fume simulate hydration; with the C/S ratios of 0.9 and 1.8 are shown in Fig. 1. Q1 silica tetrahedron structure forms at 1 day. The pozzolanic activity of silica fume is high and the amorphous silica tetrahedron structure of Q4 in silica fume reacts with calcium hydroxide to form C-S-H gel with essential Q1 silica tetrahedron structure. Q1 silica tetrahedron is active and polymerizes to Q2 silica tetrahedron structure. Therefore, the Q2 silica tetrahedron structure emerges at 3 days. The silica tetrahedron structural changes of silica fume in simulate hydration is illustrated in Fig. 2. Because there is no aluminum in silica fume, no Q2(Al) silica tetrahedron structure exists in hydration products. Moreover, as Q0 silica tetrahedron contributes is the main silica tetrahedron structure in clinker, Q2B, a bridge silica tetrahedron