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Thixotropic structural build-up is an intrinsic property of fresh cementitious materials, playing a significant role in pumpability, stability and formwork filling of concrete, as well as buildability in 3D printing. This paper presents a critical review on the thixotropic structural build-up of cement-based materials from the viewpoints of origins, evaluation methods, influencing factors and applications. Recent research indicates that the origin of structural build-up of cementitious materials is a combining result of colloidal interactions and chemical hydration, with three stages of colloidal network percolation, rigid percolation and rigidification. The evolution of static yield stress and storage modulus can be used to evaluate the structural build-up of fresh cementitious materials, each describing different aspects. Increasing particle volume fraction, decreasing surface coverage and reducing maximum packing fraction exhibit a positive effect on the increase in the structural build-up. Based on the relationships with performance parameters, the thixotropic structural build-up can be used to predict formwork casting, numerical simulations and 3D concrete printing. Furthermore, on-demand stiffening can be obtained by magneto-controlled structural build-up of cementitious materials containing magnetizable particles.

Rheology control is essential during the period in which cement and concrete pastes are encountered in the fresh state, due to the fact that it directly affects workability, initial placement and the structural performance of the hardened material. Optimizations of clinker formulations and reductions in cement-to-water ratios induced by economic and environmental considerations have a significant effect in rheology, which invokes the need for mechanistic models capable of describing the effect of multiple relevant phenomena on the observed paste flow. In this work, the population balance framework was implemented to develop a model able to relate the transient microstructural evolution of cement pastes under typical experimental conditions with its macroscopic rheological responses. Numerical details and performance are assessed and discussed. It was found that the model is capable of reproducing experimentally observed flow curves by using measured cluster size distribution information. It is also able to predict the complex rheological characteristics typically found in cement pastes. Furthermore, a spatially resolved scheme was proposed to investigate the nature of flow inside a parallel-plates rheometer geometry with the objective of assessing the ability of the model of qualitatively predicting experimentally observed behavior and to gain insight into the effect of possible secondary flows.

© 2018, The Minerals, Metals & Materials Society and ASM International. The viscosity of solid phase containing heterogeneous silicate melts is discussed in this review. The crucial parameters characterizing silicate melt structure are first presented, i.e., volume fraction of solid particles, particle shape and size. The measurement and calculation methods of these parameters are summarized and the influence of the parameters on viscosity is discussed. Next, a theoretical description of rheological behavior in heterogeneous silicate melts is given, focusing on non-Newtonian characteristics, e.g., shear-dependence, time-dependence, and yield stress. The viscosity models which were proposed in the last half century are reviewed and critically assessed. This paper concludes with opportunities and suggestions for future work. ispartof: METALLURGICAL AND MATERIALS TRANSACTIONS B-PROCESS METALLURGY AND MATERIALS PROCESSING SCIENCE vol:49 issue:5 pages:2469-2486 status: published

The refining characteristics of the highly concentrated water-in-oil emulsion, which are used as ‘emulsion precursors’ for the preparation of emulsion explosives, were investigated to elucidate the manner in which the refining time influences its microstructure and rheological behaviour. The development of microstructure at various stages of the emulsification process has been studied in detail and an empirical correlation between the characteristic droplet size and refining time has been proposed. The evolution of rheological characteristics of the emulsion during the microstructure refinement has been investigated through different protocols of the dynamic and steady-state rheology. An extended refining led to a finer microstructure and resulted in an increase in the elastic modulus, yield stress and viscosity of the emulsion. The droplet size dependency of the elasticity and the yield stress during the refining have also been discussed. The network structure of the dispersed phase, the droplet size and the corresponding interdroplet interactions all govern the rheological characteristics of the final emulsion.

WOS:000395847500002; International audience; Rheometers with specific impellers, developed to characterize the behavior of cement-based suspensions in the fresh state, are used to limit the heterogeneities induced during shearing but they make the identification of the rheological parameters less straightforward compared to conventional rheometers. This paper presents the inverse analysis method and discusses the quality of this identification procedure when applied to such materials. The procedure includes a CFD simulation based on the finite element method using a Herschel-Bulkley model. Two kinds of optimization algorithms are used: a deterministic simplex method and a stochastic genetic method. As a first step of a larger study, the procedure reported in this paper used 2D synthetic data, i.e. 2D numerically generated experimental data. Two numerical vis-coplastic materials, characterized by shear-thinning and shear-thickening, were selected and studied. The results obtained with the two algorithms are systematically compared to the known parameter solution. Three approaches corresponding to three levels of user's knowledge about the material under study are considered successively: (1) the user has no a priori knowledge about the material, (2) the user knows whether the material is shear-thinning or shear-thickening and (3) the user is able to estimate the behavior index. The time-consuming genetic method appears to be suitable when the a priori knowledge of the material is slight, whereas the simplex method gives a reliable solution in a few iterations when the level of knowledge is higher. Both algorithms encounter more difficulties with the shear-thinning material than with the shear-thickening one. In this paper, the advantage provided by the genetic method regarding the non-uniqueness of the identification procedure for real experimental data is also highlighted: this method provides a collection of satisfactory solutions among which the user can select the optimal one based on his scientific background and/or on further experimental test results.

The determination of rheological and mechanical material properties becomes a challenge when the availability of material is limited to a few (milli)grams. This miniaturized testing is hampered by the contradicting requirements of small sample sizes (and thus surface areas) and sufficiently large generated torques and forces. In this paper we provide a feasible methodology to determine the relevant material parameters in terms of processing and mechanical performance starting from 30 mg of material, using micropillars with a diameter of 1 mm. Complex viscosity in small amplitude oscillatory shear as the relevant parameter for thermoconformation processes is determined by means of eccentric rheometry. Herein, the sample is placed off-centered, which results in an increase in the generated torque without the need for increasing the size of the sample. By combining experimental data and numerical simulations, we show that the choice of the pillar aspect ratio is essential to maintain a homogeneous sample deformation and thus to extract correct rheological parameters. Values obtained with eccentric rheometry collapse with those obtained from standard rheometry. The intrinsic mechanical behavior is evaluated at room temperature and the yielding kinetics is studied. The methodology developed here can be extended to other systems and testing conditions, allowing a full material characterization in the liquid as well as in the solid state with only 30 mg of material.

Predicting the dramatic changes in mechanical and physical properties caused by irradiation damage is key for the design of future nuclear fission and fusion reactors. Self-ion irradiation provides an attractive tool for mimicking the effects of neutron irradiation. However, the damaged layer of self-ion implanted samples is only a few microns thick, making it difficult to estimate macroscopic properties. Here we address this challenge using a combination of experimental and modelling techniques. We concentrate on self-ion-implanted tungsten, the frontrunner for fusion reactor armour components and a prototypical bcc material. To capture dose-dependent evolution of properties, we experimentally characterise samples with damage levels from 0.01 to 1 dpa. Spherical nano-indentation of grains shows hardness increasing up to a dose of 0.032 dpa, beyond which it saturates. Atomic force microscopy (AFM) measurements show pile-up increasing up to the same dose, beyond which large pile-up and slip-steps are seen. Based on these observations we develop a simple crystal plasticity finite element (CPFE) model for the irradiated material. It captures irradiation-induced hardening followed by strain-softening through the interaction of irradiation-induced-defects and gliding dislocations. The shear resistance of irradiation-induced-defects is physically-based, estimated from transmission electron microscopy (TEM) observations of similarly irradiated samples. Nano-indentation of pristine tungsten and implanted tungsten of doses 0.01, 0.1, 0.32 and 1 dpa is simulated. Only two model parameters are fitted to the experimental results of the 0.01 dpa sample and are kept unchanged for all other doses. The peak indentation load, indent surface profiles and damage saturation predicted by the CPFE model closely match our experimental observations. Predicted lattice distortions and dislocation distributions around indents agree well with corresponding measurements from high-resolution electron backscatter diffraction (HR-EBSD). Finally, the CPFE model is used to predict the macroscopic stress-strain response of similarly irradiated bulk tungsten material. This macroscopic information is the key input required for design of fusion armour components.

Robustness is defined as the capacity of cement-based materials to retain fresh properties when subjected to either small variations in the constituent elements or small changes in the mixing procedure. Compared to normal concrete, self-consolidating concrete (SCC) may show less tolerance to those changes. Most robustness studies focus on initial rheological properties or workability, but concentrate less on the evolution of these properties within the first hour(s). This paper presents the results of an investigation aimed at evaluating the change of yield stress and plastic viscosity with time of cement pastes with SCC consistency, which is mainly affected by variations in the water content and the adding time of the superplasticizer. A change in water content also influences the initial rheological properties, and these differences are amplified over time. The difference due to the different adding time of the superplasticizer is, however, reduced or even reversed over time.

Soft and semisolid states of fine-grained soils and clay minerals (FGS-CMs) are frequently dealt with during execution of infrastructure projects located in the coastal areas, analysis of natural hazards, and mineral processing. In most of these cases, the FGS-CMs flow like a slurry, and hence determination of their rheological characteristics becomes essential. However, test methods and approaches available for determining the rheological behavior of the FGS-CMs when they transform from the solid to the liquid state are yet to evolve. This study uses a parallel-plate rheometer, which is widely used for rheological characterization of complex fluids (i.e., fluids which exhibit yield stress), to determine the rheological parameters (i.e.,yield stress, T-y, and strains) of the FGS-CMs with a consistency near the liquid limit. A critical analysis of the existing protocols that are used to determine T-y and their applicability to FGS-CMs is conducted. The constant shear-rate (CSR) test, when conducted at low shear-rate, yields the most accurate T-y of FGS-CMs. Subsequently, the results are used to develop a generalized relationship which explains the variation of the T-y of the FGS-CM with the consistency represented as water content normalized with respect to the liquid limit. Furthermore, to understand the nature of strains that develop during the preyielding regime of FGS-CMs, creep-relaxation (CR) tests are conducted by imposing stress equivalent to different fractions of T-y. The results from CR tests were utilized in the development of a novel methodology to determine the elastic component of the shear modulus, G(E), of FGS-CMs. This study reveals that FGS-CMs behave as a linear elastoplastic material in the preyield stage, contrary to the much expected purely elastic response, providing a new insight in the realm of contemporary geomechanics. (C) 2018 American Society of Civil Engineers.

The rheological properties of high internal phase emulsions (HIPEs), comprising polydisperse aqueous droplets in oil, have been characterized as a function of emulsification time, salt concentration, phase mass fractions and aging. The droplet size distribution and structural details of the emulsion samples were obtained using cryogenic-scanning electron microscopy (cryo-SEM) and optical microscopy. For rheological characterisation, amplitude sweep tests performed on HIPE samples with a high mass fraction of dispersed phase (93.5 wt%) show that the strain behavior, especially the yield strain ( e y ) and crossover strain ( e c ), are almost independent of the droplet size and polydispersity. However, emulsions with smaller droplets have higher yield stress ( τ y ) and storage moduli ( G ′ ) values; explanations for these observations, based on the physical properties of the systems are suggested. Furthermore, it is observed that, for constant mass fractions of oil and aqueous phases, the strain behavior is also independent of the salt concentration in the dispersed phase. Our findings indicate that, independently of the salt concentration, the energy requirement for the emulsion to start flowing is greater when smaller droplets are present. Aging studies, performed over a period of 6 months, show no significant change in the rheological properties of the HIPEs. Experimental rheology data is compared to the Princen and Kiss model, and with modified Mougel model (Ind. Eng. Chem. Res. 2011, 50, 10359–10365), giving insight into the critical effects of non-ideality induced by polydispersity in thickened emulsions.

International audience; An approach based on percolation theory is associated to the rigorousness of the two-dimensional (2D) model of close-packed, monodisperse, cylindrical emulsions established by Princen, to obtain an equation to model the dispersed-phase volume fraction (phi) dependence of the storage modulus (G') of highly concentrated emulsions. A first-order Taylor expansion of this general percolation model leads to an expression similar to the three-dimensional (3D) model proposed by Princen and Kiss for real polydisperse emulsions, with a more satisfactory derivation of the function E(phi). Finally, the robustness of this model is tested against different experimental data collected from the literature.

We investigate the time-dependent rheology and slip behaviour of colloidal gels formed under polymer-induced depletion attraction. The shape of the flow curves at low applied shear rates is suggestive of slip, which we confirm using confocal imaging. Time-dependent linear viscoelastic measurements show an unexpected drop of the elastic modulus below the viscous one after a critical time. We present a dynamic phase diagram characterizing the dependence of slip on polymer concentration and colloid volume fraction. Confocal imaging links slip to the restructuring of clusters with time, which leads to a reduction of the number of contacts between the colloidal network and the rheometer surfaces. Such behaviour is shear rate dependent and correlated to changes in the gel structure, which changed from independent small aggregates at high shear rates to percolated clusters at low shear rates.

The magneto-rheological responses of cement paste with nano-Fe3O4 particles are experimentally investigated. The estimated magneto-dynamic force between two neighboring nanoparticles and equilibrium movement velocity of the nanoparticles in cement-based suspensions are calculated. Results show that the nanoparticles have a potential to move to form magnetic clusters when a magnetic field is applied, which creates a sort of agitation effect breaking down the early C-S-H links between cement particles, and thus the corresponding suspensions exhibit liquid-like behavior immediately after applying the magnetic field. The solid-like property of the studied suspensions becomes more dominant with magnetizing time due to the formation of magnetic clusters and the reconstruction of C-S-H bridges. The rheological properties of paste medium exert significant influences on the magneto-rheological responses of cement paste containing nano-Fe3O4 particles. It is revealed that the calculated magnetic yield parameter and nanoparticle movement velocity are useful relevant indicators to evaluate the magneto-rheological effect of cementitious paste.