OSIPOV,V. I., NIKOLAEVA, K. & SOKOLOV, N. (1984). G&technique 34, No. 2, 293-303 S. V.

Microstructural

changes associated with thixotropic phenomena in clay soils

S. K. NIKOLAEVA* and V. N. SOKOLOV*

V. I. OSIPOV,

Thixotropic phenomena in clay soils are accompanied by microstructural changes. The nature of these changes is unclear because of the short duration of the thixotropic processes and the difficulties involved in preparing a specimen at certain stages. However, these technological problems were overcome and SEM photographs were obtained of the thixotropic soil microstructure during deformation of samples in a rotary viscometer with and without vibration. The new data obtained clarify the mechanism of thixotropic phenomena. Soil microstructure was not ruptured by vibration during the shear process. On the contrary, it became more homogeneous over the entire volume and at the same time this induced a decrease in strength in the system due to a reduction in cohesion at contacts. Disruption of some structural bonds is followed by their rapid restoration--the overall microstructure remaining intact. As a result, in all the samples studied the shear zone disappears. In kaolinite clay and coarser dispersed soils (silty clay, watersaturated loess) the local areas of the structural framework (shear planes) become smoother and the orientation of the structural elements along the direction of shear disappears. After the cessation of vibration, the microstructure is rapidly restored to its initial state. Les phCnom&nes thixotropiques dans les sols argilacts sont accompagnts de changements microstructurels. La nature de ces changements nest pas clair, B cause de la courte durCe des phtnombnes thixotropiques et des difficult&s de la prkparation dun Cchantillon g de certaines &tapes. Ces problkmes technologiques ont CtC rCsolus et des images SEM ont CtC obtenues de la microstructure du sol thixotropique pendant la d&formation des tchantillons dans un viscom&re rotatif avec et sans vibration. Les nouvelles donn6es obtenues clarifient le mecanisme des phtnomtnes thixotropiques. La microstructure du sol na pas 6tC rompue par la vibration pendant le cisaillement. Tout au contraire, elle est devenue plus homogkne sur le volume entier, tandis quen m&me temps ceci a cause une rCduction de la rCsistance du systkme due B une diminution de la cohCsion aux contacts. La rupture de quelques liens structurels est suivie de leur rCtablissement rapide, tandis que la microstructure entibre reste intacte. Comme rtsultat, la zone de cisaillement disparait dans tous les Cchantillons etudib. Dans largile kaolinite et les sols dispersts Discussion on this Paper closes on 1 January For further details see inside back cover. * Moscow State University. 1085.

microstructure se rCtablit rapidement dans son &at initial. INTRODUCTION

plus grossiers (argile limoneuse, loess saturC deau) les zones locales du cadre structure1 (plans de cisaillement) deviennent plus lisses, et lorientation des Cl&men% structuraux le long de la direction de cisaillement disparait. Aprts que la vibration a cessC, la

Thixotropic phenomena, exhibiting a gel-sol type of reversible isothermic transformation, are widespread in water saturated clay soils with coagulative types of structural bond, and occur upon complete remoulding (Avgustinik, 1940; Akkermann, 1948; Skempton & Northey, 1952; Gumensky, 1954; Mitchell, 1960, Gorkova, 1961; Van Olphen, 1977). The phenomena lead to unfavourable consequences: landslide activation, loss in slope stability and reduction in the bearing capacity of soil foundations. Therefore, a study of the nature of thixotropic phenomena and recognition of the characteristics of thixotropic soil behaviour is of great theoretical and practical importance in soil mechanics (Trofimov & Martynov, 1975). Thixotropic phenomena develop in structured systems and are accompanied by microstructural changes associated with thixotropic loss and restoration of strength (Ovchinnikov, Kruglitsky & Mikhaylov, 1972; Rebinder, 1979; Uryev, 1980). Hence, it is impossible to understand fully the mechanism of thixotropy without a comparative analysis of the microstructural changes that take place in a system when it is deformed under static? and dynamic conditions. The microstructural changes in clay under shear in static conditions have been studied by a investigators (Popov, number of 1944; Morgenstern & Tchalenko, 1967; Vyalov, Pekarskaya & Maksimyak, 1970; McKeys & Yong, 1971; Tovey, 1971. However, the characteristics of these changes during deformation with applied vibration have received little attention: this is because of the technical difficulties

*The term characterize

static conditions soil deformation

is used in this Paper without vibration.

to

293

294 Table 1. Description 0,055 0.01 mm Characteristics

OSIPOV, NIKOLAEVA of the soils studied Granulometric O.Ol0.005 mm composition: 0.0050.001 mm %

AND SOKOLOV

Mineral composition of the clay fraction mm

co.002

Moisture content at liquid limit W,: % 56 200 40

Clay Clay Silty clay

2 2 29

21 21

30 31

47 97 19

L.oess

16

11

Kaolinite Montmorillonite (100%) Illite (40%) mixed-layered (30%), chlorite (20%), kaolinite (7%), montmorillonite (3%) Illite (60%), mixed-layered (20%), kaolinite (lo%), chlorite (10%)

25

associated with the high sensitivity of thixotropic soils, and the complexity of the rapid fixation of the microstructure at various stages in the thixotropic transformation. The Authors have obtained new experimental data which provide a better understanding of thixotropic phenomena. EXPERIMENTAL Soils studied PROGRAMME

Soil samples of variable dispersion and mineral composition were used to study the characteristics of microstructural changes associated with thixotropic phenomena. Monomineral clays (kaolinite and montmorillonite) and polymineral silty clays and loess were used (Table 1). The experiments were performed on reconstituted paste samples prepared at moisture contents ranging from O.SW, to 2.2W,, where W, is the moisture content at the liquid limit. In this state the samples had a typical coagulation structure characteristic of the majority of modern and poorly lithified clay soils. The samples were thoroughly mixed with distilled water and the resulting paste was placed in a desiccator with a container of water for about 24 hours. This allowed the moisture in the paste to become uniform without changing in value. Thereafter the paste was used in the experiments, with moisture content and temperature under constant control. Shear tests. To characterize the thixotropic behaviour of the prepared samples, their resistance to shear was studied in static conditions and with applied vibration. Tests were performed during continuous shear deformation by employing a rotary viscometer, Reotest-2, with the cylinder measuring device mounted on a vibrostand (Fig. 1). To reduce the impact of

normal stresses and near-the-wall slip, hollow measuring cylinders with knurled surfaces were used in the experiments. The pastes were placed in the 3 mm wide ring gap of a coaxial cylinder system. The external cylinder of the viscometer was rigidly fixed on the electrodynamic vibrostand, which served as a source of harmonic vertical vibration. The internal cylinder revolved at a constant velocity of 1 rev/min. The following vibration parameters were used in the experiments: frequency 20 Hz, displacement amplitude 0.6 mm, acceleration 10 m/s, duration 5 min. This set of conditions corresponds to the conditions for the majority of dynamic soil problems of interest, e.g. those induced by earthquakes or by traffic (Puchkov, 1974; Pavlenkov, 1978). Measurements of the rotary moment value on

Fig. 1. Diagram of the rotary viscometer, Reotest-2.1 internal cyfinder wtth kmuled surface; 2 external cylinder; 3 paste in the gap between the internal and external cylinders; 4 liqaid nitrogen container for sample freezing; 5 vibrostand; w angle speed; f frequency of the vibration

THIXOTROPIC

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Static

Pynami4

Static

Fig. 2. Shear resistance (7) against time (t) relationship for soil subjected to static and dynamic shear conditions: OA shear resistance of the ondisturbed stmctore under static conditions; AB shear resistance for the roptored stroctore (residual strength); CD shear resistance of the ruptured stroctore wlth vibration; EF shear resistance of the thixotropically restored structure (after cessation of vibration); BC drastic drop in strength (with vibration) and DE strength restoration (after cessation of vibration). 0, 1, 2, 3 soil sample selection points for microstractoral
StUdieS

the internal cylinder axis were taken at various known deformation velocities. Calculation of the shear resistance (T) was performed with the use of the following relation (Uryev, 1980): M r=zz where M is the rotative moment, L is the height of the internal cylinder immersed in the clay paste and r is the radius of the internal cylinder. A static shear test was begun and performed at a constant deformation velocity of 2.5 X 10m4 m/s, which corresponds to conditions of rapid shearing. After a constant shear resistance value (residual resistance) was set up the vibrator was switched on. Five minutes later the vibrator was switched off and shearing deformation continued in the absence of external vibration. The shear resistance recorded is shown in Fig. 2 as a function of time for the staticdynamic-static test sequence. The figure suggests that the vibration disrupts the structural bonds, causing the soil strength to be significantly reduced. To examine the microstructure at any stage of the test the microstructure had to be fixed as rapidly as possible while the test was in progress. This was done by pouring liquid nitrogen into the container surrounding the soil sample and the gap between the internal and external cylinders (see Fig. l), while simultaneously stopping the test. Because the sample thickness was only about 3 mm, freezing was essentially instantaneous. It is considered that no change in the

microstructure was caused by this freezing process. The apparatus was disassembled to remove the frozen soil sample. Portions of the sample were selected for moisture removal by sublimation in a vacuum chamber-the process is known as freeze-drying (Barden & Sides, 1977; Tovey, Frydman & Wong, 1973; Smart & Tovey, 1982). In this technique very rapid freezing is used in an attempt to solidify the soil porewater instantaneously without disruptive crystal growth. Subsequently, sublimation under vacuum removes the ice without disturbing the microstructure of the soil. Details of the freeze-drying procedure are well described by Smart & Tovey (1982). Three identical samples of each paste were prepared and tested. One was frozen after constant shearing resistance was achieved, corresponding to the condition at point 1 in Fig. 2. The second was frozen during vibration (point 2, Fig. 2), and the third was frozen at maximum strength after the cessation of vibration (point 3, Fig. 2). A fourth identical sample was prepared and then frozen without shearing. This sample represented the initial microstructure. Microstructural studies of samples after freeze-drying were performed with the aid of the scanning electron microscope (CWIKSCAN106). The most interesting peculiarities of microstructure were photographed at a number of magnifications (from Xl00 to x10 000). The images obtained were used for assessing the qualitative and quantitative characteristics of microstructural changes in the portions of interest on the shear curve. Quantitative microstructural analysis was performed with the aid of the image analyser. This analysis provided information on the pore area, the distribution of pores and microaggregates by size and the orientation of the soil microstructural elements inside and outside the shear zone (Sergeyev, GrabowskaOlszewska, Osipov & Sokolov, 1980).
MICROSTRUCTURAL OBSERVATIONS

Initial paste microstructure The specimens from the montmorillonite paste had a honeycomb microstructure (Fig. 3(a)), typical of a fine-grained clay system with high water content (Sergeyev et al., 1980). This microstructure is characterized by interaction between the montmorillonite microaggregates of the face-toface and face-to-edge type, with the development of closed, predominantly isometrically shaped cells with diameters ranging from fractions of a micron to 2-3 km. (Fig. 3(a), A, C, D).

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velopment of shear planes-local disruptions of the structural framework. Outside the shear zone the orientation of the structural elements is absent and the clay microstructure is similar to that of the kaolinite initial sample (Fig. 4(a)). Evaluation of the kaolinite paste pore area disclosed that its value within the shear zone comprises 68%, and beyond the shear zone 58%. Marked orientation of the structural elements is also characteristic of coarse-grained systemsthe silty clay and loess pastes. Referring to Fig. S(c), at contacts the grains and clayey substance become orientated along the shear direction, although a marked shear plane is absent here. Increasing porosity in the shear zone is observed in coarse-grained systems, as for montmorillonite and kaolinite pastes. Microstructural changes under dynamic shear Applying vibration during the shearing process leads to considerable microstructural changes in the samples studied. The vibration of the montmorillonite paste makes for a more regular honeycomb microstructure (Fig. 4(c)) in comparison with that of the initial structure (Fig. 4(a)), with cells as a rule not more than 1.52.5 urn in diameter. The decrease in size of the microaggregates is observed as a result of their disruption by vibration. It is important to note that with applied vibration the shear zone disappears. A similar effect is observed with kaolinite paste; the vibrational impact leads to elimination of the orientation of structural elements along the shear direction, and the shear zone also disappears. In this case the microstructure becomes more homogeneous through the entire specimen (Fig. 5(c)). The quantitative pore area estimation of the photographs produced by the image analyser (Sergeyev et al., 1980) shows that the pore area in a kaolinite paste actually does not change when it is removed from the internal to the external viscometer cylinder, and comprises on average 62%. The gross changes in the microstructure of the silty clay and loess pastes that take place with applied vibration result in a more homogeneous and regular honeycomb microstructure. At the same time, oscillation of the coarse sandy and silty grains in these soils disturbs their structure, making it less cohesive. SEM photographs taken after the impact of vibration on soils appear to show that the vibration brings about disruption of the clay bridges (Fig. 5(d)). Microstructural changes upon cessation of vibration The cessation of vibration (during shear de-

formation) is followed by a process of rapid reversal which restores the microstructure: microaggregate size increases, with the formation of larger and less homogeneous pores. Thus, for instance, in montmorillonite paste the size of the pores approaches 2-3 pm. Pores regain their initial size, and the total pore area comprises 53%. The SEM photographs (Figs 3(a), (d); 4(a), (d); 5(a), (e)) show the similarity of the microstructure before and after the cessation of vibration, The clay bridges are restored between the sandy and silty grains in silty clay and loess pastes (Fig. 5(f)). DISCUSSION Microstructural investigations of thixotropic processes in clay soils have shown soil strength under static and dynamic shear to be dependent on microstructural changes. Under static shear the soils studied react immediately to shear stress by displaying minor displacements. At this stage reversible elastic deformations dominate, as a result of the partial tilting of particles and microaggregates in the direction of the shear force without displacement relative to one another (Tshukin & Rebinder, 1971). Load removal at this stage of deformation leads to elastic restoration with time of the initial state of particle arrangement. As the maximum strength of a test sample r,, (Fig. 1) is approached and deformation increases, the elastic deformation gradually changes to viscoplastic in the narrow shear zone, leading to rebuilding of the soil microstructure in this zone. In the case of the fine-grained systems such as the montmorillonite paste, the rebuilding is manifested through partial microaggregate disruption resulting in a more regular honeycomb microstructure in the shear zone. In the case of coarser systems formed by isometric microaggregates of a plate type (e.g. kaolinite paste), reorientation of the microaggregates also occurs along the direction of shear stress. Both processes are followed by an increase in soil porosity in the shear zone, the development of negative pore pressure and an increase in moisture content (Skempton, 1974; Smolin, 1977; Meschan, 1978). A number of large sized pores elongated to the shear zone are formed besides (Fig. 6, part B). The development of similar pores (canals) in the shear zone is evidently connected with intensive moisture migration to the deformed zone under the impact of negative pore pressure. This originates as a result of decreasing density and increasing porosity in the soil in the shear zone. Microstructural rebuilding and the development of a shear zone bring about a reduction in growth for the strength of

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the system during continuous deformation, with the value r reaching its maximum and then beginning to decline. A transfer over maximum (the structural strength limit) is explained by the formation of a shear zone with weakened structural bonds between the particles and the microaggregages, a result of the increased moisture content and partial reorientation of the structural elements along the shearing force direction. However, some investigators are inclined to attribute this to breaking up of the spatial structural framework into separate blocks (Abduragimova, Rebinder & Serb-Serbina, 1955; Uryev, 1980). The portion AB of the graph (Fig. 2) shows progressive development of the shear zone, accompanied by a further increase in porosity and orientation of the structural elements, enhancing soil moisture content within the zone and reducing strength. The progress of deformation leads to completion of the shear zone development and stabilization of the shear stress, expressed by the appearance of a horizontal portion on the deformation graph (residual strength T,,,.). Microstructural studies of samples at this stage of deformation show the existence of a clearly defined shear zone, whose width at the plane shear of plastic clays changes from a few microns to a few millimetres. The experiments prove that the width of the soil shear zone grows while the microaggregate size decreases and the moisture content of the soil increases. The impact of vibration under dynamic shear leads to a drastic reduction in the shear resistance of soils (portion BC on the shear curve, Fig. 2), depending on the vibration parameters, and remaining permanent up until the cessation of impact (portion CD on the shear curve, Fig. 2). Some investigators explain this phenomenon by the complete structural disruption and loss of structural cohesion (Trofimov & Martynov, 1975), others consider that vibration facilitates particle orientation in the direction of a shear displacement, thus causing a reduction in the strength of a system (Lishtvan, Bityukov & Terentyev, 1977). The microstructural studies carried out suggest that the joint action of shear force and vibration results, not in rupture, but, on the of a more contrary, in the development homogeneous microstructure over the entire sample volume. A dynamic state is induced in a soil by the impact of a vibration field as a result of the forced oscillation of particles and their microaggregates. The structural elements are displaced, structural cohesion weakens and partial disturbance of microaggregates and an increase in soil dispersion takes place. The relative

mobility of the structural elements grows and the relaxation processes are accelerated. A more homogeneous microstructure appears along the entire gap of the viscometer, and the shear zone disappears, probably because of reorientation of the structural elements and their interaction within the most energetically advantageous areas. The orientation of the structural elements along the direction of shear force disappears because the vibration displacement gradient exceeds the velocity gradient of shear deformation. Cessation of vibration leads to rapid restoration of the soil structure. This is shown by the fast growth of the shear strength of soils some seconds after vibration has ceased, and by the occurrence of a second maximum on the shear curve (portion DE of the shear curve, Fig. 2). A drastic increase in soil strength upon cessation of vibration is caused by the mutual fixation of particles and the creation of coagulation contacts between them. As a result, over the volume a structural framework is formed in the specimen, characterized by the uniform distribution of the water in the entire specimen. This process is attended by an increase in the size of microaggregates and the formation of a less homogeneous porosity. The soil microstructure formed is similar to the initial microstructure. Rapid restoration of the soil strength at rest is followed by a further strengthening which continues for a long period of time. This is because, in a soil after vibration, the establishment of thermodynamic equilibrium is related to the microstructural changes, which are not accomplished instantaneously, but proceed for a certain period of time until the thixotropic restoration of the system is complete. CONCLUSION The studies have given a more complete view of the microstructural changes that take place in thixotropic soils during deformation in a rotary viscometer with and without vibration, thus providing a deeper insight into the mechanism of thixotropic phenomena. The data obtained indicate that without vibration clay deformation occurs over a limited volume-in the shear zoneand is attended by marked changes in the soil microstructure in this zone: i.e. a decrease in the size of the microaggregates and the diameter of the predominant pores, a decrease in the density of the system and an increase in moisture content. These microstructural changes are directly related to the value of the maximum and minimum shear strengths of the soils. It is important to note that, under shear test, for the system composed of small-sized particles (gener-

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ally less than a micron, i.e. montmorillonite) the deformation in the shear zone is volumetric in character, and does not lead to disruption of structural continuity (shear planes). It is obvious that the mechanism of deformation in such systems is relaxational or thixotropic, i.e. the microstructure-forming cells are ruptured at shear, and at the same time are instantaneously restored, without forming a linear defect in the in addition to the microstructural changes described above, in a shear zone the microaggregates become orientated along the direction of shear stress and local shear planes develop, along which the orientation of structural elements is particularly marked. For these soils during shear therefore both volumetric deformation and local disruption of the structural framework occur along developing shear planes. Observations indicate that vibration applied during the shearing process does not disrupt the microstructure; on the contrary, it becomes more homogeneous over the entire volume, as a result of a reduction in cohesion at contacts. The loosening of the structural bonds between particles and microaggregates during vibration promotes disruption of large microaggregates and more uniform stress distribution along the entire gap of the viscometer. It also accelerates the relaxation processes and facilitates the mutual reorientation of particles and microaggregates. In these systems disruption of some structural bonds is followed by rapid restoration, with the overall microstructure remaining intact. This results in the disappearance of the shear zone in all the samples studied. In kaolinite paste and coarser dispersed soils (silty clay, loess) the local areas of the structural framework (shear planes) become smooth and the orientation of the structural elements along the direction of shear disappears. The deformation spreads over the volume compared with the situation during shear before vibration is applied. The cessation of vibration is followed by rapid of the existing spatial structural fixation framework at the expense of strengthening of the coagulation contacts due to speed, causing a drastic increase in soil strength some seconds after switch-off. Concurrently with strengthening of the system, a number of processes lead to an enlargement of the microaggregates and a reduction in porosity. As a result, the clay microstructure after thixotropic soil restoration shows a similarity to its initial state before the shear tests. A subsequent increase in thixotropic soil strength with time is evidently related to the thermodynamic establishment of gradual equilibrium and complete restoration of the initial microstructure.
structure. olinite), In coarser dispersed clayey soils (ka-

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Skempton, A. W. & Northey, R. D. (1952). The sensitivity of clays. Gtotechnique 3, No. 1, 3053. Smart, P. & Tovey, N. K. (1982). Electron microscopy of soils and sediments: techniques, pp 51-55. Oxford: Clarendon Press. Smolin, Yu. P. (1977). A study of the pore pressure in soil at shear moment. Trans. Novosibirsk Inst. Railway Engrs, No. 180, 89-91. Tovey, N. K. (1971). A selection of scanning electron micrographs of clays. CUED/C-soil/TRSa, pp 2-4. University of Cambridge. Department of Engineering, Tovey, N., Frydman, S. & Wong, K. Y. (1973). A study of swelling clay in the scanning electron microscope. Froc. 3rd lnt. Con?. Expansive Soils, Haifa. pp 45-54. Trofimov, V. T. & Martynov, A. P. (1975). On the

quicksands and thixotropic properties of silty soils in the seasonally thawing layer of the Yamal peninsula. Natural Conditions of Western Siberia, No. 5, 256-263. Tjumen (in Russian). Tshukin, E. D. & Rebinder, P. A. (1971). On the mechanism of the elastic after-effect in structurized bentonite suspensions at minor concentration. Colloid J. 33, No. 3, 450-458 (in Russian). Uryev, N. B. (1980). Highly concentrated fine-grained systems, chap. 5, pp 173-190 Moscow: Khimia (in Russian). Van Olphen, H. (1977). An introduction to clay colloid chemhy (2nd edn), pp 138-139. New York. Yvalov, S. S., Pekarskaya, N. K. & Maksimyak, R. V. (1970). On the physical essence of the deformation and disruption processes in clay soils. Fountains and Soil Mechanics, No. 1, 7-9. Moscow (in Russian).