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The flowability of cement paste is of great importance in today’s construction industry and is influenced by additives such as superplasticizers (SP). One type of SPs are polycarboxylate ether type SPs. These additives electrostatically bind with the negatively charged carboxylic groups at the backbone to the positively charged clinker phases.
To model positively charged clinker phases with adsorbed SP, silicon Wafers are pre-coated with cationic polyethylenimine (PEI) and SP is adsorbed onto the coated surface (Si/PEI/SP). Two different polycarboxylate ether type (PCE) SP are compared – one for ready-mix concrete and one for precast concrete. In this preliminary study the interaction forces between Si/PEI/SP surface and a silica microsphere (colloidal probe) are investigated under mild physico-chemical conditions (pH *6, ion concentration <10−5 M) using Colloidal Probe Atomic Force Microscopy (CP-AFM).
The interaction force between the model surfaces is attractive for low concentration of SP. The force changes from attractive to repulsive by increasing amount of SP. The force upon approach reveals a biexponential behavior. The exponential decay at large and short surface separations are attributed to electrostatic and steric interactions, respectively. The steric forces of the SP for ready-mix concrete show a steeper onset than the SP for precast concrete.
The quantification of these interaction forces will be compared to rheological measurements of similar systems. Furthermore, the parameters will be changed to better approach the conditions in real systems, i.e. higher pH and ionic strength. This helps to understand how the forces on the nanoscale influence the macroscopic rheology.
Viscosity modifying agents: Key components of advanced cement-based materials with adapted rheology
(2022)
Viscosity modifying agents (VMAs) are essential ingredients for the production of flowable cement-based materials. This paper presents an overview of commonly used VMAs and attempts to shed some light on the underlying physics at the origin of their mechanisms of action. The main molecular parameters of VMA controlling the rheological properties of the cement pore solution are highlighted. As the mechanisms of action of VMAs in cement-based materials are closely related to their affinity with the surface of cement particles, the adsorption of the main VMA types is discussed. The effect of VMAs on flow properties and stability of cement-based materials is presented for VMAs added without any superplasticizer, and then in systems incorporating both VMAs and superplasticizers. Finally, the effect of VMAs in enhancing concrete properties to secure adequate performance of different construction applications, and perspectives for future developments of novel cement-based materials made with VMAs are showcased.
The presence of polycarboxylate ether (PCE) based superplasticizers (SPs) has enormous influence on the early hydration of cement. C3A as the most reactive phase of Portland cement plays a significant role in early hydration reactions and affects the rheological performance. Therefore, this paper presents experimental results about the influence of delayed addition of PCEs on the Hydration of cement and C3A-gypsum pastes investigated by isothermal heat flow calorimetry. Complementary in-situ XRD was carried out on C3A pastes to analyze hydration and phase changes related to the addition of PCE.
Cement pastes with a delayed addition of PCE showed less Retardation compared to simultaneous addition. The alteration caused by PCE is much more pronounced for C3A-gypsum mixes. With a delayed addition of SP, the hydration of C3A is less retarded or even accelerated. It is obvious that there is less retardation the later the addition of SP. Furthermore, the PCE alter the hydration of C3A when added delayed and exhibit changes in kinetics and hydration rates. XRD results showed that more C3A is dissolved in the presence of PCE. Also, the gypsum depletion occurs earlier in the presence of PCE and even faster with delayed addition. Without PCE AFm starts to form just after the gypsum depletion. However, in the presence of PCE AFm already starts to form at the beginning of the hydration. Due to the faster gypsum depletion in the presence of PCE, also the transformation from ettringite into AFm begins earlier, but takes longer as without SP.
The presence of polycarboxylate ether (PCE) based superplasticizers (SPs) has an enormous influence on the early hydration of cement. The hydration is retarded and the timing of formation and the morphology of hydrates is affected. This short paper presents experimental results about the influence of delayed addition time of PCE SPs on hydration of cement and alite pastes, investigated by isothermal heat flow calorimetry. For cement as well as for alite pastes the hydration is retarded with SP, whereby the high charge PCE has a stronger retarding effect than the low charge PCE. The retardation caused by PCE is much more pronounced for alite than for cement mixes. If PCE is added later to the mix, the induction period is shortened and the hydration is accelerated compared to simultaneous addition. This applies for cement and alite pastes. With delayed PCE addition the alite shows a clearly less retarded setting and main hydration than after simultaneous addition. It is obvious that for alite pastes there is less retardation the later the addition of SP.
The presence of polycarboxylate ether (PCE) based superplasticizers (SPs) has an enormous influence on the early hydration of cement. The hydration is retarded and the timing of formation and the morphology of hydrates is affected. This short paper presents experimental results about the influence of delayed Addition time of PCE SPs on hydration of cement and tricalcium aluminate (C3A) pastes, investigated by isothermal heat flow calorimetry. For cement pastes the hydration is retarded with SP, whereby the high charge PCE has a stronger retarding effect than the low charge PCE. With delayed PCE addition the cement shows a less retarded setting than with simultaneous addition. The alteration caused by PCE is much more pronounced for C3A and gypsum mixes than for cement. If the SP is added simultaneous, the exothermic peak of C3A is retarded. However, with delayed addition of SP the hydration is shortened, the gypsum depletion is fastened and the exothermic peak occurs less retarded or even accelerated compared to simultaneous addition. It is obvious that for C3A pastes there is less retardation the later the Addition of SP. Furthermore, the PCE alter the hydration of C3A when added delayed and exhibit changes in kinetics and hydration rates. The rate of reaction in the second stage is lower, discernible in decreased slopes and broader peaks. Besides this, a distinct ramp in the C3A heat flow curves within the first stage of C3A hydration occurs for all pastes with delayed addition of SP, which suggests an accelerated ettringite formation.
Admixtures are important constituents to enhance the performance of concrete. They allow for more efficient use of binders which can mitigate negative environmental impacts from producing cement-based materials. Commonly used rheology modifying agents like polycarboxylate ethers or cellulose ethers are synthetic or semi-synthetic, respectively. This requires additional energy consumption for their production and global supply chains particularly for many developing regions, which will be large consumers of concrete in the future. However, many locally available bio-based polysaccharides could be effectively used instead. These polymers are often overlooked by engineers and scientists due to their limited distribution and inherent complexity, yet they represent an underleveraged source of precursors for admixtures. This study investigates the action mechanisms of some bio-based rheology modifying agents, i.e., acacia gum and miscanthus gum, and provides a comparison to a conventionally modified starch. The results show that the mechanism of action of these polymers is closely related to the composition of the mixture, mixing regime, and the composition of the aqueous phase. Depending on the agent, either plasticizing or stabilizing effects on rheology can be revealed.
In this paper, we demonstrate the value of 1H NMR relaxometry for studying the hydration of clinker-reduced, more climate-friendly cementitious binders. The results were obtained on typical CEM I cements and sister samples containing two different reactive agricultural ashes as well as non-reactive biochars as supplementary cementitious materials. The findings prove that time-resolved NMR measurements provide valuable additional information when combined with classical heat flow calorimetry.
Special applications like pumping, spraying or printing of concrete require the precise adjustment of very specific rheological properties at different time steps during the casting process. Superplasticizers such as polycarboxylate ethers (PCE) can be used to obtain the required flowability, which, possibly in combination with additional rheology modifying admixtures, generate the required specified consistency. However, after the application, the concrete should change the rheological properties immediately in order to avoid deformations at rest. Therefore, the use of accelerators can be effective. Accelerators influence the hydration of cementitious materials, and thus the rheological properties over the course of time and the setting.
In this paper, the influence of different accelerators on the rheology and early hydration of cement paste as well as the interaction of accelerator and PCE are presented. Methods like rheometry, needle penetration tests and practical Tests like spread flow were applied. The used accelerators showed accelerating behavior on the cement pastes without and in the presence of PCE. At the same time an influence on the rheology could be observed. This effect was less in the mixes with PCE, especially at the highest water/cement ratio (w/c).
In the last years flowable concrete has become increasingly important in applications such as, for systems with highly reinforced concrete with a complicated formwork, or sprayed concrete and 3D-printing of concrete. For all these applications it is necessary to have tailored rheological properties. Rheology can be described by values of yield stress and plastic viscosity, which can be determined for example by evaluation of rheometer measurements. But for different materials various rheometers with different geometries and stirrers are being used. To see the effects from paste in concrete, it is necessary to investigate mixes of paste, mortar and concrete, stepwise. But currently there exists no device, which is calibrated for these different systems at once. Due to this fact, conventional tests such as V-funnel efflux-time and flow diameter were determined, as well as rheometer data in different cell sizes and geometries.
In this study the assessment of rheological effects in the binder on the rheology of mortar and concrete was investigated by using combination of two rheometers.
Die Rheologie von fließfähigen zementären Systemen mit Fließmitteln wird durch eine Vielzahl parallel stattfindender Effekte beeinflusst. Zu diesen Effekten zählen Wechselwirkungen zwischen den Polymeren und Ionen in der Porenlösung, frühe Phasenbildung, zeitabhängige und kompetitive Adsorption zwischen anionischen Polymeren und Sulfationen, Bildung von Phasen in der Porenlösung sowie Morphologieänderungen an Partikeloberflächen. Die frühe Hydratation von Zement, die durch Lösungs- und Fällungsprozesse angetrieben wird, beeinflusst diese Effekte erheblich. Das permanente Ungleichgewicht der Porenlösung führt zu Veränderungen der Partikeloberflächen, welches widerum zur Folge hat, dass rheometrische Messungen dieser Zementleime anfällig für Streuungen sind. Um die Einflüsse aus der Zementhydratation zu minimieren, wurden die rheometrischen Untersuchungen mit Zement in Porenlösung durchgeführt. Die Experimente wurden mit verschiedenen Feststoffvolumenfraktionen durchgeführt und mit den Ergebnissen identischer Systeme mit Wasser anstelle von Porenlösung verglichen. Zusätzlich wurden die gleichen Systeme mit Zugabe von Polycarboxylatethern untersucht.
Die Ergebnisse zeigen, dass die Leime mit Wasser niedrigere Werte für Fließgrenze und plastische Viskosität aufweisen, als die Systeme mit Porenlösung. Während die Polymere eine Verminderung der Fließgrenze zur Folge hatte, war die Wirkung von Polymeren auf die plastische Viskosität vernachlässigbar. Zusätzlich wurde die frühe Hydratation unter Verwendung von Wärmeflusskalorimetrie, Rasterelektronenmikroskopie und Nadeleindringtiefe beobachtet.