Experimental Study of Micro Behavior of Hangzhou Soft Clay Jieqing Huang Research Center of Coastal and Urban Geotechnical Engineering, Zhejiang University, Hangzhou, Zhejiang, 310058, China e-mail: [email protected] Xinyu Xie * Research Center of Coastal and Urban Geotechnical Engineering, Zhejiang University, Hangzhou, Zhejiang, 310058, China *Corresponding Author, e-mail: [email protected] Jinzhu Li School of Civil Engineering & Architecture, Ningbo Institute of Technology, Zhejiang University, Ningbo, Zhejiang, 315100,China e-mail: [email protected] Wenjun Wang School of Civil Engineering & Architecture, Ningbo Institute of Technology, Zhejiang University, Ningbo, Zhejiang, 315100,China e-mail: [email protected] ABSTRACT One-dimensional (1D) oedometer, mercury intrusion porosimetry (MIP) and scanning electron microscopy (SEM) tests are performed on Hangzhou soft clay samples to research the micro mechanical characteristics. Based on 1D oedometer tests, it can be found that the secondary consolidation behavior of Hangzhou soft clay is obvious. Moreover, two Hangzhou soft clay samples show the tertiary consolidation behavior. It can be found from MIP results that the compression of soft clays preferentially occurs in the weaker interaggregate pores instead of in the stronger intraaggregate pores during both primary and secondary consolidation. It can be observed from SEM images that the arrangement of clay particles becomes more orderly and the pores become smaller with developing consolidation. KEYWORDS: Hangzhou soft clay; one-dimensional oedometer test; mercury intrusion porosimetry test; scanning electron microscopy imaging INTRODUCTION Natural rocks or soils, generally have certain microstructures developed during depositional processes. Some scholars have demonstrated that microstructure is directly attributed to properties of natural deposits [1-3]. Generally, there are three types of fabric associations in soft clays: edge-to-edge(EE) flocculation, edge-to-face(EF) flocculation and face-to-face(FF) aggregation [4-5]. Different types of fabric associations form different types of pores. In general, the pores in soft clays can be divided into interaggregate pores and intraaggregate pores. The - 6105 - Vol. 19 [2014], Bund. U 6106 interaggregate pores refer to the space between the aggregates while the intraaggregate pores refer to the space inside the aggregates [2,6]. Some scholars proposed the dual-porosity hypothesis with associated delays of water expulsion [7-9]. This hypothesis assumes that primary consolidation comes from the dissipation of the pore water pressure in the interaggregate pores, and secondary consolidation occurs when water discharges from the intraaggregate pores. Many efforts have been made to research the dual-porosity hypothesis. Nevertheless, this hypothesis has been proven inadequate in some existing experiments [10-11]. The controversy regarding the rationality of this hypothesis continues today. Hangzhou soft clay is widely deposited on the plains of Hangzhou and it can cause the excessive settlement of buildings because of high compressibility. Many scholars did research on the macro properties of Hangzhou soft clay. The soften of normally consolidated Hangzhou soft clay under cyclic loading was studied by cyclic triaxial tests with stress-controlled [12]. Comprehensive tests on Hangzhou intact soft clay were performed to obtain the soils’ critical response to undrained dynamic stress paths under different combinations of principal stress orientation [13]. Based on undrained cyclic triaxial tests, the cyclic behaviors of Hangzhou soft clay subjected to initial shear stress were investigated [14]. Nevertheless, the micro behavior of Hangzhou soft clay is yet to be investigated. In this paper, a series of experiments using one-dimensional (1D) oedometer tests, mercury intrusion porosimetry (MIP) and scanning electron microscopy (SEM) are performed on Hangzhou soft clay samples to research the micro mechanical characteristics and reexamine the dual-porosity hypothesis. Firstly, MIP and SEM tests are carried out on natural Hangzhou soft clay samples to study the natural pore-size distribution and observe some representative pores and clay particles. Afterwards, 1D oedometer tests are performed on Hangzhou soft clay samples. Then MIP tests are performed to characterize the pore-size evolution of Hangzhou soft clay in the process of consolidation. Finally, with the help of SEM, the microstructure evolution of Hangzhou soft clay during consolidation can be observed clearly. EXPERIMENTAL DETAILS Sample preparations Some undisturbed block samples of Hangzhou soft clay and Hangzhou stiff clay were obtained in Zijingang Campus of Zhejiang University. Then oedometer tests were carried out in the oedometer room in the same campus. Hangzhou stiff clay is selected herein for comparison purposes. The basic properties of Hangzhou soft clay and Hangzhou stiff clay are summarized in Table 1. Table 1: Basic index properties of Hangzhou soft clay and Hangzhou stiff clay Properties Specific gravity Gs Saturated unit weight γsat(kN/m3) Natural water content w(%) Natural void ratio e Plastic limit wP(%) Liquid limit wL(%) Hangzhou soft clay 2.67 17.74 44.86 1.18 20.0 41.2 Hangzhou stiff clay 2.65 19.30 13.05 0.55 18.6 34.2 Vol. 19 [2014], Bund. U 6107 Experimental procedures 1D oedometer test The 1D oedometer tests are divided into two portions: multi-stage loading tests and singlestage loading tests. Multi-stage loading tests are performed on two Hangzhou soft clay samples. The first loading is 25 kPa. Then the applied load is increased to 50, 100, 200, 400, 800 and 1,600 kPa. In the test of sample 1, each applied load is maintained for 24 hours. The test of sample 2 aims to observe the secondary consolidation behavior of Hangzhou soft clay under each applied load. In this test the amount of time to allow the development of secondary consolidation is one week. The information of multi-stage loading tests is summarized in Table 2. Sample 0 represents the natural Hangzhou soft clay sample in this paper. Table 2: Information of multi-stage loading tests Sample number Duration of each loading stage(hours) Final loading(kPa) 0 0 0 1 24 1600 2 168 1600 In the single-stage loading tests, two kinds of samples are investigated: Hangzhou soft clay and Hangzhou stiff clay. Hangzhou stiff clay is investigated for comparison purposes. Six samples are investigated and they are divided into three sets. In each set, there is one Hangzhou soft clay sample and one Hangzhou stiff clay sample and the two samples are applied with the same load. The applied loads of three sets are 100 kPa, 200 kPa and 300 kPa respectively. The consolidation is considered finished when the vertical settlement becomes completely steady. The information of single-stage loading tests is summarized in Table 3. SOFT and STIFF represent Hangzhou soft clay and Hangzhou stiff clay in this table respectively. Table 3: Information of single-stage loading tests Sample number Kind of sample 3 SOFT 4 STIFF 5 SOFT 6 STIFF 7 SOFT 8 STIFF Applied load(kPa) 100 100 200 200 300 300 After the 1D oedometer tests, the samples are carefully trimmed into small cubes. These cubes are immediately put into liquid nitrogen and then they are freeze dried. The freeze-dried cubes are then used for the MIP tests and SEM imaging. MIP test The MIP test is based on the principle that a non-wetting liquid cannot enter a porous medium unless forced under external pressure. Considering the pores as cylindrical capillary tubes, the intrusion pressure P and the pore diameter D are related as follows [15]: D = −4 γ cos θ / P (1) where γ=surface tension of mercury and θ=the contact angle between clay minerals and mercury. The value of γ has been consistently reported to be 0.484 N/m [2, 16]. However, an accurate value ofθ is difficult to obtain because this angle is intimately related to the properties of clay Vol. 19 [2014], Bund. U 6108 minerals. Diamond [17] determined a contact angle of 139°for montmorillonite and 147°for other clay minerals. Penumadu and Dean [18] measured the contact angle of mercury with kaolin clay and they found the advancing and receding contact angles are equal to 162°and 158°respectively. Based on Diamond’s recommendation, the value of θ is equal to 147°in this study. The AutoPore IV 9510 with a maximum intrusion pressure of 414 MPa is used in the MIP analysis and it is shown in Fig. 1. The range of pore-size measurements is from 0.003 µm to 360 µm. SEM imaging Some representative cubes, after freeze-drying and gold coating, are selected for SEM imaging. The thermal field emission SEM used in this research is shown in Fig. 2. Its type is SIRION-100 and it is produced by FEI in Holland. The maximum magnification is 100000. Figure 1: Mercury intrusion porosimetry Figure 2: Thermal field emission scanning Electron microscopy EXPERIMENTAL RESULTS Microstructure of natural Hangzhou soft clay Fabric associations and pore types in soft clay Wang and Xu [11] classified the pores in soft clays into four categories: Type A, Type B, Type C and Type D. This classification is applied in this paper. Type A pores are the small intraaggregate pores between the clay particles in the aggregates. Note that the intraaggregate pores mentioned in the dual-porosity hypothesis are referred to as Type A pores [9,19,20]. Type B pores are the large intra-aggregate pores and they can have a wide range of sizes [11]. In natural soft clays, there are EE or EF associations between clay particles. Type C pores are formed within this weak structure. Type D pores lie in the structure formed by aggregates, so they Vol. 19 [2014], Bund. U 6109 are stronger than Type C pores. It is worth mentioning that Type D pores are the interaggregate pores mentioned in the dual-porosity hypothesis. The conceptual view of soft clays is shown in Fig. 3. Four types of pores can be clearly observed. It can be seen that a clay particle is of a plate shape and several particles are gathered in a group, forming an aggregate, together with interlayer water. Based on SEM results, the length and width of a clay particle are generally within the range of 1~10µm and the thickness of a clay particle is approximately 1µm. EE flocculation Type C pore EF flocculation FF aggregation Type D pore Type B pore Type A pore (a) Microscopic structure of soft clays 1µm~10µm clay particle ¡Ö 0.1µm Type A pore (b) an aggregate of clay particles Figure 3: Conceptual view of soft clays Pore-size distribution MIP tests are performed on natural Hangzhou soft clay (sample 0) and the test results are shown in Fig. 4. It can be observed that the pore size distribution of natural Hangzhou soft clay has two sharp peaks: the major peak located at a diameter of about 0.1 µm and the minor peak located at a diameter of about 100 µm. It is clear that the major peak represents the intraaggregate pores and the minor peak represents the intera-ggregate pores. According to the aforementioned classification of pores, the major peak indicates the Type A pore and the minor peak indicates the Type D pore. It is evident that Types A and D pores are the dominant pores in natural Hangzhou soft clay. It is worth mentioning that MIP analysis does not give the measurement of pore sizes, but of pore entrance sizes. Delage and Lefebvre [2] pointed out that MIP analysis may give smaller average values for relatively large pores. Vol. 19 [2014], Bund. U 6110 Figure 4: Pore size distribution of natural Hangzhou soft clay Representative pores The pores in natural Hangzhou soft clay samples are observed by performing the SEM tests. The SEM images in Fig. 5 provide details of several representative pores. Fig. 5(a) shows a special pore which is composed of two Type D pores: an outer pore and an inner pore. It is shown that both of the outer and inner pores are formed by aggregates. The sizes of these two pores are approximately 1.5µm×1.5µm and 0.5µm×0.75µm respectively. The pore shown in Fig. 5(a) is a nested pore and it is named Type D-D pore in brief. The pore shown in Fig. 5(b) is also special because it is formed by an individual clay particle and some aggregates. As mentioned, Type C pores and Type D pores are formed by clay particles and aggregates respectively. This special pore is named the composite pore. A representative Type B pore is shown in Fig. 5(c) and its size is approximately 1µm×3µm. The aforementioned classification of pores is based on the structure of pores and it is strict. Nevertheless, it can be found from Fig. 5 that the majority of actual pores in Hangzhou soft clay are irregular. Sometimes it is difficult to classify an actual pore into a certain type. Vol. 19 [2014], Bund. U (a) Type D-D pore 6111 (b) Composite pore (c) Type B pore Figure 5: SEM images of pores in natural Hangzhou soft clay Representative clay particles Fig. 6 presents three SEM images of clay particles in natural Hangzhou soft clay. Fig. 6(a) shows the top view of aggregated structures composed of hundreds of clay particles. It can be observed that the clay particles have a wide range of sizes and they are arranged unevenly. Fig. 6(b) shows several close-ups of dispersed clay particles. The clay particle in the lower left portion of this figure seems like a rectangle and its size is approximately 1.5µm×2.5µm. In order to measure the thickness of clay particle, we observe the side view of aggregated structures. It can be seen from Fig. 6(c) that the thickness of clay particle is about 0.1 µm and the width of Type A pore is about 0.1 µm too. Vol. 19 [2014], Bund. U (a) Top view of aggregated structures 6112 (b) Dispersed clay particles (c) Side view of aggregated structures Figure 6: SEM images of clay particles in natural Hangzhou soft clay Microstructural evolution of Hangzhou soft clay in response to consolidation 1D oedometer results Multi-stage loading tests are performed on two Hangzhou soft clay samples. As noted, for sample 1 and sample 2, the amounts of time to allow the consolidation development under each applied load are one day and one week respectively. The e-logp curves (e=the void ratio and p=the consolidation stress) of the two samples are plotted in Fig. 7. The difference between the void ratios of the two samples under each applied load shows the amount of secondary compression. It can be observed from Fig. 7 that the above difference is 0.1 under 25 kPa load and it becomes 0.2 under 1600 kPa. This implies that the accumulative secondary compression increases with increasing applied load. Vol. 19 [2014], Bund. U 6113 Figure 7: Oedometer compression curves MIP results As mentioned, MIP tests were performed on sample 1 and sample 2 after consolidation. The pore-size distribution curves of samples at three different stages, i.e., the initial stage (sample 0), the stage after primary consolidation (sample 1) and the stage after secondary consolidation (sample 2), are jointly considered in Fig. 8. It can be observed that the amount of the minor peak apparently decreases during both primary and secondary consolidation. However, the major peak remains almost unchanged during consolidation. This observation implies that the aggregated structure that encloses Type A pores moves as a whole during consolidation. Considering the characteristics of the Types A and D pores, the Type D pores are more collapsible than the Type A pores because the EF or EE contacts have much smaller areas compared with those at the FF contacts and small contact areas can lead to a higher stress concentration. It can be found that the compression of soft clays preferentially occurs in weaker Type D pores during both primary and secondary consolidation. Hence, the secondary consolidation is fundamentally the same as the primary consolidation. Vol. 19 [2014], Bund. U 6114 Figure 8: Pore size distributions of Hangzhou soft clay samples at different consolidation stages SEM results Fig. 9 shows the SEM images of sample 0, sample 1 and sample 2. The magnification of these three SEM images is 5000. It can be observed from Fig. 9(a) that in the natural sample the arrangement of clay particles is disorderly and there are many large Type D pores. It can be found from Fig. 9(b) that after primary consolidation large pores disappear but medium and small pores still exist in the sample. It can be seen from Fig. 9(c) that after secondary consolidation the arrangement of clay particles is much more orderly than before. At this time, the majority of pores are Type A pores. (a) Initial stage (sample 0) (b) Stage after primary consolidation (sample 1) Vol. 19 [2014], Bund. U 6115 (c) Stage after secondary consolidation (sample 2) Figure 9: SEM images of Hangzhou soft clay samples at different consolidation stages Microstructural evolution of Hangzhou soft clay in response to secondary consolidation 1D oedometer results Single-stage loading tests are performed on three Hangzhou soft clay samples and three Hangzhou stiff clay samples. The experimental results are shown in Fig. 10. It can be observed that the final settlement of Hangzhou soft clay sample is much larger than that of Hangzhou stiff clay sample under the same load. Moreover, the settlement of Hangzhou stiff clay sample is increasing approximately linearly all the time without secondary consolidation behavior. Nevertheless, the settlement of Hangzhou soft clay sample increases quickly at first and then increases slowly after the first inflection point. In conclusion, the settlement of Hangzhou soft clay is large and the secondary consolidation behavior of Hangzhou soft clay is very obvious. (a) 100 kPa (b) 200kPa Vol. 19 [2014], Bund. U 6116 (c) 300kPa Figure 10: Time-deformation curves of Hangzhou soft clay samples and Hangzhou stiff clay samples under different consolidation pressures For the Hangzhou soft clay samples under 100kPa and 200kPa loads (sample 3 and sample 5), the settlement rates increase after the second inflection point. It can be observed that the clay exhibits secondary and tertiary consolidation. Ichikawa et al. [20] found that bentonite shows the tertiary consolidation. They considered that the chemical properties of soils are drastically changed if multicharged anions are infiltrated in the last stage of consolidation. They thought that the above mechanism causes the change of permeability and then causes the tertiary consolidation. Nevertheless, their opinion was not based on experimental results. When the settlement becomes completely steady, we open the specimens exhibiting the tertiary consolidation and find some changes. First, all of the samples have an intense rotten smell; Second, the natural color of Hangzhou soft clay is light gray, but some dark-gray-colored stains are found at the surfaces of the samples; Third, the erosion of the filters is severe and many small holes appear on the filters. According to the above phenomena, we conjecture that humus exists in the natural Hangzhou soft clay. The permeability of soils changes when the humus causes a series of chemical reactions in the last stage of consolidation. Unfortunately, further chemical or biological analyses are not performed on the samples to investigate the inner components of humus and the mechanism of the chemical reactions. The relationship between humus and tertiary consolidation is yet to be investigated. The ending times of primary consolidation tp under different applied loads are judged with the Casagrande Method. Afterwards, the secondary compression indices Cα during two different periods under different applied loads are calculated. The calculation results are summarized in Table 4. It can be seen that tp decreases with increasing applied load and Cα decreases with increasing time under each applied load. Table 4: Secondary consolidation parameters of Hangzhou soft clay samples Parameters tp(minutes) Cα(tp-1000 minutes) Cα(1000-10000 minutes) 100 70 0.01303 0.00690 Applied load (kPa) 200 300 55 50 0.01140 0.00998 0.00514 0.00427 Vol. 19 [2014], Bund. U 6117 MIP results The MIP analyses were carried out on the three Hangzhou soft clay samples after secondary consolidation. The experimental results are shown in Fig. 11. It can be observed that the minor peak gradually decreases but the major peak remains almost unchanged with increasing applied load. This implies that the compression of soft clays mainly occurs in weaker Type D pores instead of the stronger Type A pores. Figure 11: Pore size distributions of Hangzhou soft clay samples after secondary consolidation Even though the observations in Fig. 8 and Fig. 11 can not verify the dual-porosity hypothesis, this hypothesis should not be completely abandoned. The expulsion of water from the intraaggregate pores still can account for the deformation of soft clays during secondary consolidation. Nevertheless, the expulsion of water from the interaggregate pores is much more significant than that from the intraaggregate pores. SEM results Fig. 12 presents the SEM images of the three Hangzhou soft clay samples after secondary consolidation. The magnification of the SEM images is 5000. Jointly considering the three SEM images, it can be easily observed that with increasing applied load, the arrangement of clay particles becomes more orderly and the pores become smaller and smaller. Vol. 19 [2014], Bund. U (a) 100 kPa (sample 3) 6118 (b) 200 kPa (sample 5) (c) 300 kPa (sample 7) Figure 12: SEM images of Hangzhou soft clay samples after secondary consolidation CONCLUSIONS In this paper, the 1D oedometer, MIP and SEM tests are carried out on Hangzhou soft clay samples to investigate the change in macromechanical and microstructural behavior during consolidation. The following conclusions can be made: 1) In natural Hangzhou soft clay, types A and D pores are the dominant pores. The majority of actual pores are irregular and it is difficult to classify an actual pore into a certain type. 2) Hangzhou soft clay samples all exhibit the secondary consolidation behavior clearly. Two Hangzhou soft clay samples show the tertiary consolidation behavior. The relationship between humus and tertiary consolidation is yet to be researched. 3) The compression of soft clays preferentially occurs in the weaker interaggregate pores instead of in the stronger intraaggregate pores during both primary and secondary consolidation. This implies that the secondary consolidation is fundamentally the same as the primary consolidation. Vol. 19 [2014], Bund. U 6119 ACKNOWLEDGEMENTS The writers would like to thank Dr. Jie Song in the research and teaching lab for civil and hydraulic engineering in Zhejiang University for her help in the 1D oedometer tests. We would also like to thank Dr. Qun Pu in the state key laboratory of chemical engineering in Zhejiang University for her help in the MIP tests. Dr. Mingyong Yuan in the analysis and measurement center of Zhejiang University is acknowledged for his help in the SEM imaging. The financial supports from National Natural Science Foundation of China under approved No. 51378469, Zhejiang Provincial Natural Science Foundation of China under approved No. Y1111240 and Natural Science Foundation of Ningbo City, China under approved No. 2013A610196 are gratefully acknowledged. REFERENCES 1. Mesri, G., Rokshar, A., Bohar, B. F., (1975) “Composition and compressibility of typical samples of Mexico City clay.” Géotechnique, 25(3), 527-554. 2. Delage, P., Lefebvre, G., (1984) “Study of the structure of a sensitive Champlain clay and of its evolution during consolidation.” Canadian Geotechnical Journal, 21(1), 21-35. 3. Diaz-rodriguez, J. A., Lozano-santa, C. R., Davila-alcoce, V. 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