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At least 1,081 records · Page 60
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DOE OSTI2013

Sulfate attack expansion mechanisms

A specially constructed stress cell was used to measure the stress generated in thin-walled Portland cement mortar cylinders caused by external sulfate attack. The effects of sulfate concentration of the storage solution and C{sub 3}A content of the cement were studied. Changes in mineralogical composition and pore size distribution were investigated by X-ray diffraction and mercury intrusion porosimetry, respectively. Damage is due to the formation of ettringite in small pores (10–50 nm) which generates stresses up to 8 MPa exceeding the tensile strength of the binder matrix. Higher sulfate concentrations and C{sub 3}A contents result in higher stresses. The results can be understood in terms of the effect of crystal surface energy and size on supersaturation and crystal growth pressure.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Observations on dedolomitization of carbonate concrete aggregates, implications for ACR and expansion

Some carbonate aggregates used in concrete are unstable in a high alkaline solution, which is present also in pore solution of cement binder. This paper investigates the process of dedolomitization of carbonate aggregate rocks and mortar bars. Selected aggregates, limestone and dolostone are of high purity without reactive silica involvement confirmed by the XRD and the XRF. For the process of dedolomitization the effect of various temperatures, solutions and time was examined. In this investigation, measurements of expansion, optical and scanning electron microscopy (SEM), energy dispersive spectrometry (EDS) and X-ray diffraction were used. Te results indicate that the process of dedolomitization occurred not only in the NaOH solution but also in the water on the mortar bar with virgin dolostone aggregate. Elevated temperature, 60 °C, increased the rate of reaction. Furthermore, the rate of reaction significantly correlates with time, which has also been confirmed through the Rietveld analysis. -- Highlights: •The dedolomitization caused no expansion. •It occurs in the dolostone aggregate without reactive silica involvement. •It has taken place already with the presence of the cement binder. •A significant alteration occurred: formation of rims, new pores and phases.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Hydration mechanisms of two polymorphs of synthetic ye'elimite

Ye'elimite is the main phase in calcium sulfoaluminate cements and also a key phase in sulfobelite cements. However, its hydration mechanism is not well understood. Here we reported new data on the hydration behavior of ye'elimite using synchrotron and laboratory powder diffraction coupled to the Rietveld methodology. Both internal and external standard methodologies have been used to determine the overall amorphous contents. We have addressed the standard variables: water-to-ye'elimite ratio and additional sulfate sources of different solubilities. Moreover, we report a deep study of the role of the polymorphism of pure ye'elimites. The hydration behavior of orthorhombic stoichiometric and pseudo-cubic solid-solution ye'elimites is discussed. In the absence of additional sulfate sources, stoichiometric-ye'elimite reacts slower than solid-solution-ye'elimite, and AFm-type phases are the main hydrated crystalline phases, as expected. Moreover, solid-solution-ye'elimite produces higher amounts of ettringite than stoichiometric-ye'elimite. However, in the presence of additional sulfates, stoichiometric-ye'elimite reacts faster than solid-solution-ye'elimite.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Applying high resolution SyXRD analysis on sulfate attacked concrete field samples

High resolution synchrotron X-ray diffraction (SyXRD) was applied for a microstructural profile analysis of concrete deterioration after sulfate attack. The cement matrices consist of ordinary Portland cement and different amounts of supplementary cementitious materials, such as fly ash, natural pozzolana and granulated blast furnace slag. The changes of the phase composition were determined along the direction of sulfate ingress. This approach allows the identification of reaction fronts and zones of different phase compositions and conclusions about the mechanisms of sulfate attack. Two reaction fronts were localized in the initial 4 mm from the sample surface. The mechanism of deterioration caused by the exposition in the sulfate-bearing soil is discussed. SyXRD is shown to be a reliable method for investigation of cementitious materials with aggregates embedded in natural environments.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Degradation processes of reinforced concretes by combined sulfate–phosphate attack

A novel form of alteration due to the interaction between hydrated cement phases and sulfate and phosphate-based pollutants is described, through the characterization of concrete samples from an industrial reinforced concrete building. Decalcification of the cement matrices was observed, with secondary sulfate and phosphate-based mineral formation, according to a marked mineralogical and textural zoning. Five alteration layers may be detected: the two outermost layers are characterized by the presence of gypsum–brushite solid solution phases associated with anhydrous calcium sulfates and phosphates, respectively, while a progressive increase in apatite and ammonium magnesium phosphates is observable in the three innermost layers, associated with specific apatite precursors (brushite, octacalcium phosphate and amorphous calcium phosphate, respectively). The heterogeneous microstructural development of secondary phases is related to the chemical, pH and thermal gradients in the attacked cementitious systems, caused by different sources of pollutants and the exposure to the sun's radiation.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Influence of the Ca/Si ratio of the C–S–H phase on the interaction with sulfate ions and its impact on the ettringite crystallization pressure

The effect of the Ca/Si ratio of the calcium–silicate–hydrate (C–S–H) phase on the interaction with sulfate ions is investigated for C–S–H phases (Ca/Si = 0.83, 1.25, 1.50) and mortar samples of blended Portland cements. It is shown that leaching of calcium from C–S–H and portlandite affects the composition of the pore solution and contributes to the developing crystallization pressure of ettringite. Sulfate profiles show that sulfate binding before cracking is similar for different Ca/Si ratios whereas the highest expansion rates are observed for the mortars with the highest Ca/Si ratios. After leaching in sulfate solutions, the C–S–H samples have been characterized by {sup 29}Si MAS NMR, thermogravimetric analysis, and elemental solution analysis. Generally, the exposure to sulfate solutions results in decalcification of the C–S–H, which increases with decreasing Ca/Si ratio. The data are in good agreement with thermodynamic modeling, indicating that equilibrium is almost achieved in the leached systems. Finally, the expansion of mortar samples exposed to sulfate solutions was much less at lower Ca/Si ratios of the cement blends. This reduced expansion can be related to the decrease of the supersaturation of the pore solution with respect to ettringite at lower Ca/Si ratios of the C–S–H and in the absence of portlandite.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Observing the setting and hardening of cementitious materials by X-ray dark-field radiography

Novel X-ray imaging methods expand conventional attenuation-based X-ray radiography by the phase- and the dark-field contrasts. While weakly absorbing structures in the specimen can be better visualized in phase contrast, the dark-field contrast provides information about morphological sub-pixel microstructures. Here we report an application of dark-field X-ray radiography for imaging the time-resolved setting process in fresh cement. Our results demonstrate that the microstructural changes within the cement result in a decreasing dark-field signal. We quantify this imaging signal with a time-dependent dark-field scatter coefficient and show its good correlation with the compressional wave velocity. We further present images based on a pixel-wise analysis of the scattering signal and a corresponding logistic fit. These images emphasize the benefit of dark-field imaging of cementitious materials as it provides two dimensional spatial information on the processes within the sample while other established testing techniques only provide information on the bulk average.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Direct three-dimensional observation of the microstructure and chemistry of C{sub 3}S hydration

Disagreements about the mechanisms of cement hydration remain despite the fact that portland cement has been studied extensively for over 100 years. One reason for this is that direct observation of the change in microstructure and chemistry are challenging for many experimental techniques. This paper presents results from synchrotron nano X-ray tomography and fluorescence imaging. The data show unprecedented direct observations of small collections of C{sub 3}S particles before and after different periods of hydration in 15 mmol/L lime solution. X-ray absorption contrast is used to make three dimensional maps of the changes of these materials with time. The chemical compositions of hydration products are then identified with X-ray fluorescence mapping and scanning electron microscopy. These experiments are used to provide insight into the rate and morphology of the microstructure formation.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Vegetable ashes as Supplementary Cementitious Materials

Approximately 140 billion metric tons of biomass are produced every year in the world from agriculture. The ashes resulting from firing agricultural wastes such as rice husk, sugar cane and others can be used as Supplementary Cementitious Materials (SCM). They can be mixed with lime alone or in ternary mixtures with Portland cement and lime. If fired at temperatures around 600–700 °C the agricultural ashes exhibit good reactivity. Despite extensive research work carried out on the use of agricultural ashes as source of SCMs, few success stories are reported on practical applications on an industrial scale. Details of the firing technology should be re-assessed, with special emphasis on the scale at which the technology begins to be economically suitable. Further research is also needed to understand the mechanisms of structural transformation of amorphous silica during calcination, and the impact of the ashes on cement hydration in blended systems.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Hydrate failure in ITZ governs concrete strength: A micro-to-macro validated engineering mechanics model

Ever since the early days of Féret (1892) and Abrams (1919), concrete research has targeted at relating concrete composition to uniaxial compressive strength. While these activities were mainly characterized by empirical fitting functions, we here take a more fundamental approach based on continuum micromechanics. The loading applied at the concrete level, is first concentrated (''downscaled'') to maximum stresses related to cement paste volumes which are directly adjacent to the aggregates, i.e. to the interfacial transition zones (ITZ). These maximum stresses are further ''downscaled'' to the micron-sized hydrates, in terms of higher-order stress averages. The latter enter a Drucker-Prager failure criterion with material constants derived from nanoindentation tests. The model is successfully validated across the hydrate-to-concrete scales. Strength magnitude is governed by ITZ stress concentrations, and the water-to-cement ratio is its dominant mixture design parameter.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural packing- and rheology-based binder selection and characterization for Ultra-high Performance Concrete (UHPC)

This paper reports strategies to design the binder phase of ultra-high performance concretes (UHPC) from commonly available cement replacement (fly ash, slag, microsilica, metakaolin) and fine filler (limestone) materials. A packing algorithm is used to extract the number density, mean centroidal distance, and coordination number of the microstructure. Similarly, rheological studies on the pastes provide yield stress, plastic viscosity, and min-slump spread. The selection criteria involves using the three microstructural and three rheological parameters individually or in combination to define packing and flow coefficients. The selection criteria is flexible enough to allow users modify the constraints depending on the application. In this study, only ternary and quaternary blends, with a total cement replacement of 30% by mass are selected for further characterization. The highly efficient microstructural packing in these mixtures and better workability that facilitated dispersion of particles to enhance the reactivity results in beneficial pore structure and mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Impact of the microstructure model on coupled simulation of drying and accelerated carbonation

During carbonation, the microstructure of a cement paste is strongly modified, which induces a dynamic feedback loop impacting the global advancement of the reaction. In this study, we investigate the effect of the microstructure model on simulations of accelerated carbonation of cement pastes. A variable-porosity reactive transport model with a new microstructure model is used. To match the chemical layers created by the carbonation front, we use a layered microstructure model. We demonstrate that qualitative prediction for a large range of conditions and formulations can only be obtained if the macroscopic parameters of the carbonated layer can be modelled accurately. In particular, the saturation dependent parameters, such as the capillary pressure or the relative diffusion coefficients, control the rate of advancement of the reaction front since a high saturation inhibits the carbon dioxide diffusion.

36 MATERIALS SCIENCE↗
DOE OSTI2018

An atomistic building block description of C-S-H - Towards a realistic C-S-H model

Understanding the atomistic structure of Calcium silicate hydrate (C-S-H), the main product of cement hydration, is of paramount importance to better formulate sustainable cement. The existing atomistic models are not in total agreement with experimental results and fail to explain the nanosized nature of C-S-H. Here, we present a new approach for describing the complexity of these structures at the molecular level, enabling a detailed comparison of C-S-H models. The new methodology encodes a full, large scale atomistic C-S-H structure by a simple, readable string of characters, similar to the way the base sequence in DNA encodes a vast range of different proteins. We then use the methodology to assess 14 Å tobermorite-defect structures and their stabilities using DFT and classical molecular dynamics. Finally we highlight how the model may be extended to develop reliable atomistic C-S-H models for a range of Ca/Si ratios and conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Key mechanisms controlling internal curing performance of natural fibers

Since the physical and chemical characteristics of wood pulps are complex, their behaviors in a cementitious matrix are difficult to capture by conventional techniques. Here, in situ NMR/MRI along with isothermal calorimetry and surface characterization methods are used to obtain new insights into the internal curing mechanisms of hardwood pulp-cement composites. It found that eucalyptus pulps release free water in their lumen structure within 25 h of hydration. Beyond 25 h, mostly free water in small cell wall pores and bound water in the cell wall are responsible for mitigation of the ongoing self-desiccation during continued cement hydration. Sorption results suggest that chemical wood pulps behave like a semi-permeable membrane, in which the greatest binding occurs for the most abundant cation. Surface analysis reveals discrete precipitates on the pulp surface, suggesting that it may facilitate nucleation of hydration products.

36 MATERIALS SCIENCE↗
DOE OSTI2018

The composition and performance of alite-ye'elimite clinker produced at 1300 °C

Alite-ye'elimite clinker is a high cementing clinker prepared by introducing calcium sulfoaluminate, a non-silicate mineral, into the cement clinker. The mineral composition and mechanics of tricalcium silicate-rich sulfur aluminate prepared at 1300 °C are reported. The effects of copper slag and phosphorus slag on the phase composition, heat release and compressive strength were investigated. The phase composition was analysed by X-ray powder diffraction. The results show that the copper slag and phosphorus slag can lower the burn temperature of the clinker and promote the coexistence of C{sub 3}S and C{sub 4}A{sub 3} S-bar . The quality of clinker produced at 1300 °C is satisfactory. The compressive strength of mortar curing at 28 d is higher than that of P·II 52.5.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Acceleration of OPC by CAC in binary and ternary systems: The role of pore solution chemistry

In dry-mortar-formulations calcium aluminate cement (CAC) is often used as a set accelerator for ordinary Portland cement (OPC). However, a critical amount of CAC is able to delay not only the silicate reaction but also the renewed C{sub 3}A dissolution of an OPC. This delay can be counteracted by adding an appropriate amount of calcium sulfate (C$) to the mix OPC/CAC. The initial hydration period is dominated by fast ettringite formation from CA (CAC) and CaSO{sub 4} from OPC generating early strength. High aluminum and low calcium concentrations in the pore solution probably hinder C-S-H seeding and precipitation, thus preventing alite dissolution. Aluminum has to be initially removed by precipitating hydrate phases to change the pore solution chemistry. The start of the silicate reaction is then induced by increasing the calcium concentration in the pore solution.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Understanding the hydration of dolomite in cementitious systems with reactive aluminosilicates such as calcined clay

This study investigates the hydration of dolomite, CaMg(CO{sub 3}){sub 2}, with calcined clay in presence of calcium hydroxide and ordinary Portland cement. The hydration products as well as the microstructure at various ages were characterized using X-ray diffraction (XRD), thermogravimetric analysis (TGA), and mercury intrusion porosimetry (MIP). Isothermal calorimetry was used to understand the reaction kinetics. The systems with dolomite were compared against control systems with limestone and quartz. It was seen that, the formation of carbonate – AFm phases takes place in the dolomite systems similar to limestone systems. No formation of brucite (Mg(OH){sub 2}) was observed till 90 days of hydration, with Mg{sup 2+} ions most likely being incorporated into hydrotalcite phase (Mg{sub 4}Al{sub 2}(OH){sub 14}). The synergetic effect observed in the Portland cement – calcined clay – dolomite system was found to result in a refined pore structure at early ages and improvement in the mechanical properties such as compressive strength.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Combined curing as a novel approach to improve resistance of ultra-high performance concrete to explosive spalling under high temperature and its mechanical properties

Highlights: • The combined curing can significantly enhance the resistance of UHPC to explosive spalling under high temperature. • The combined curing can improve the mechanical properties of UHPC remarkably. • Both further hydration of residual cement and pozzolanic reaction are activated under a high temperature steam condition. - Abstract: The influence of a combined curing composed of precuring in hot water and heating in dry air on mechanical properties and explosive spalling of ultra-high performance concrete (UHPC) subjected to high temperature was investigated in this experiment. Meanwhile, the microstructure of UHPC was determined by means of X-ray diffraction (XRD) with Rietveld method, thermogravimetric analysis (TGA), scanning electron microscope (SEM) and mercury intrusion porosimetry (MIP). The results indicate that the combined curing improves the mechanical properties of UHPC remarkably. More importantly, it is quite efficient to enhance the resistance of UHPC to explosive spalling under high temperature, which should be a novel approach to prohibit spalling occurrence, different from adding polypropylene fiber. During dry air heating in the combined curing, a high temperature steam environment is established in the dense structure framework of UHPC formed in the preceding hot water curing. Both further hydration of residual cement and pozzolanic reaction of mineral admixtures can be activated during the dry air heating, leading to not only the formation of a large amount of dense hydrates (such as C-S-H gels, katoite, tobermorite and xonotlite, etc.), which accumulate in the aforementioned existing framework, but also the consumption of most of internal free water. Therefore, both mechanical properties of UHPC and its resistance to explosive spalling under high temperature can be enhanced significantly.

36 MATERIALS SCIENCE↗