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At least 505 records · Page 28
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DOE OSTI2016

In situ synchrotron powder diffraction study of the setting reaction kinetics of magnesium-potassium phosphate cements

This work reports a kinetic study of the formation of magnesium-potassium phosphate cements accomplished using in-situ synchrotron powder diffraction. The reaction: MgO + KH{sub 2}PO{sub 4} + 5H{sub 2}O → MgKPO{sub 4} · 6H{sub 2}O was followed in situ in the attempt of contributing to explain the overall mechanism and assess the influence of periclase (MgO) grain size and calcination temperature (1400-1600 °C) on the reaction kinetics. Numerical kinetic parameters for the setting reaction have been provided for the first time. The best fit to the kinetic data was obtained using a weighted nonlinear model fitting method with two kinetic equations, representing two consecutive, partially overlapping processes. MgO decomposition could be described by a first order (F1) model followed by a Jander diffusion (D3) controlled model. Crystallization of the product of reaction was modelled using an Avrami model (A{sub n}) followed by a first order (F1) chemical reaction. A reaction mechanism accounting for such results has been proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Prediction of water vapour sorption isotherms and microstructure of hardened Portland cement pastes

Water vapour sorption isotherms of cementitious materials reflect the multi-scale physical microstructure through its interaction with moisture. Our ability to understand and predict adsorption and desorption behaviour is essential in the application of modern performance-based approaches to durability analysis, along with many other areas of hygro-mechanical and hygro-chemo-mechanical behaviour. In this paper, a new physically based model for predicting water vapour sorption isotherms of arbitrary hardened Portland cement pastes is presented. Established thermodynamic principles, applied to a microstructure model that develops with hydration, provide a rational basis for predictions. Closed-form differentiable equations, along with a rational consideration of hysteresis and scanning phenomena, makes the model suitable for use in numerical moisture simulations. The microstructure model is reconciled with recently published {sup 1}H NMR and mercury intrusion porosimetry results.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Effect of retarders on the early hydration of calcium-sulpho-aluminate (CSA) type cements

The retardation of calcium-sulpho-aluminate (CSA) type cements by three common retarders—sodium gluconate, sodium–potassium tartrate and borax is investigated at a 2% addition rate. Each of the retarders has a different effect on the early-age hydrate assemblage, as shown by quantitative X-ray diffraction, thermogravimetric analysis, scanning electron microscopy and pore solution analysis. Regardless of the retarder used, the hydration starts with mainly the dissolution of ready soluble (calcium) alkali sulphates and ye'elimite, followed by the formation of ettringite and aluminium hydroxide, whereby the specific clinker mineral dissolution as well as ettringite-forming reaction is delayed in different ways depending on the retarder used. The results showed that the retardation is mainly caused by preventing hydrates formation in the case of tartrate and gluconate. Contrary, borax retards the hydration by preventing to a certain extent the dissolution of ye'elimite and lowers the initial pH. Furthermore, the morphology of ettringite is altered depending on the type of the retarder used.

36 MATERIALS SCIENCE↗
DOE OSTI2016

A {sup 1}H NMR relaxometry investigation of gel-pore drying shrinkage in cement pastes

The first systematic study of the temporal evolution of the pore-size-distribution (PSD) in mature cement pastes following one and two cycles of drying and rewetting is presented. The PSD is measured using {sup 1}H nuclear magnetic resonance (NMR) relaxometry. For millimetre sized paste samples dried fairly strongly, the volume of water taken up shortly after rewetting slightly exceeds the pre-drying amount. The volume of water in pores > 10 nm far exceeds that in smaller pores. This reverses the situation observed prior to drying. Over subsequent days the water distribution reverts to its original form, so that the dominant fraction is again in the smaller pores. Since the total water content scarcely changes, this indicates a re-arrangement of the nano-scale porosity. Over two drying–rewetting cycles, both reversible and irreversible changes are seen. The effect is not observed in moderately dried pastes.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Berlinite substitution in the cement clinker

Incorporation of P{sub 2}O{sub 5} in clinker minerals in laboratory samples of clinker with graded content of P{sub 2}O{sub 5} were studied by means of electron microscopy. The most important outcome is that P{sub 2}O{sub 5} enters partially the structure of clinker silicates together with Al{sub 2}O{sub 3} via berlinite substitution (Al{sup 3+} + P{sup 5+} ↔ 2 Si{sup 4+}). Therefore, experiments were also carried out with the pure components and the influence of P{sub 2}O{sub 5} on clinker phase composition in the absence of one of the main clinker oxide (Fe{sub 2}O{sub 3} and Al{sub 2}O{sub 3}) was examined. It was found out that raw mix without Fe{sub 2}O{sub 3} eliminates to a certain level negative influence of P{sub 2}O{sub 5} on alite formation. The work was completed with preparation of white cement with high content of P{sub 2}O{sub 5} in clinker, which exhibited good technological properties.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Mineralization dynamics of metakaolin-based alkali-activated cements

This paper investigates the early-age dynamics of mineral formation in metakaolin-based alkali-activated cements. The effects of silica availability and alkali content on mineral formation were investigated via X-ray diffraction and solid-state {sup 29}Si magic-angle spinning nuclear magnetic resonance spectroscopy at 2, 7, 14, and 28 days. Silica availability was controlled by using either liquid- (immediate) or solid-based (gradual) sodium silicate supplements. Mineral (zeolitic) and amorphous microstructural characteristics were correlated with observed changes in bulk physical properties, namely shrinkage, density, and porosity. Results demonstrate that, while alkali content controls the mineralization in immediately available silica systems, alkali content controls the silica availability in gradually available silica systems. Immediate silica availability generally leads to a more favorable mineral formation as demonstrated by correlated improvements in bulk physical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Hydration behavior of magnesium potassium phosphate cement and stability analysis of its hydration products through thermodynamic modeling

Magnesium potassium phosphate cement (MKPC) is normally applied in civil engineering because of its short setting time and superior mechanical properties. This study investigates the hydration behavior and hydration products of MKPC influenced by molar ratio between magnesia and phosphate (M/P ratio) through thermodynamic method. Results show that the composition of ultimate hydration products are controlled by concentration of KH{sub 2}PO{sub 4} and MgO, activity of water and pH value of solution. When M/P ratio is lower than 0.64, the hydration product is MgHPO{sub 4}·3H{sub 2}O; When M/P ratio is between 0.64 and 0.67, the hydration products are MgHPO{sub 4}·3H{sub 2}O and Mg{sub 2}KH(PO{sub 4}){sub 2}·15H{sub 2}O. When M/P ratio is between 0.67 and 1.00, hydration products are Mg{sub 2}KH(PO{sub 4}){sub 2}·15H{sub 2}O and KMgPO{sub 4}·6H{sub 2}O; When M/P ratio is higher than 1.00, the hydration product is KMgPO{sub 4}·6H{sub 2}O together with unreacted MgO. This study also investigated the effect of additives, namely B(OH){sub 3}, H{sub 3}PO{sub 4}, K{sub 2}HPO{sub 4} and KH{sub 2}PO{sub 4}. - Highlights: • A database particularly for MKPC system at 25°C, 0.1 MPa was established and verified. • The pH value corresponding to specific M/P ratio in MKPC system is successfully predicted at 25°C, 0.1 MPa. • The composition of hydration products influenced by M/P ratio and some additives is successfully predicted at 25°C, 0.1 MPa.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Phase assemblage of composite cements

The phase assemblage of binary Portland cements with 45 wt% replacement by calcareous fly ash and slag has been investigated by experiment, mass balance and thermodynamic simulations. The input for these calculations was based on clinker reaction measured by XRD-Rietveld refinement, on SCM reaction measured by SEM-EDS full element mapping and on C-S-H composition by SEM-EDS point analyses. A sensitivity analysis estimates the uncertainty of determination of phase volume as at best ± 2 cm{sup 3}/100 cm{sup 3}, and thus of rather semi-quantitative character. The differences between experiment and calculations regarding AFt/AFm, C-S-H and portlandite were assessed. Gel/space ratios computed using the volumes of all hydrates showed a clear correlation to compressive strength, which was unaffected by the mix composition. This suggests that the type of hydrates formed has little or no influence on the compressive strength and that the key factor is the space filling.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Predictive modelling of hydration and mechanical performance of low Ca composite cements: Possibilities and limitations from industrial perspective

We quantified hydration and performance development of composites cements containing metakaolin in the rage of 0–40% and investigated applicability of thermodynamic and micromechanical models to predict the evolution of hydrates assemblage and of performance, respectively. The reaction of metakaolin results in a formation of significant amounts of C-S-H phase for lower metakaolin content and of strätlingite for higher contents. This leads to very dense matrix with finer porosity allowing co-existence of thermodynamically incompatible phases, namely portlandite and strätlingite. Hence, thermodynamic modelling cannot be applied to correctly predict the phase assemblage for the systems with high metakaolin content. By introducing constraints into the thermodynamic model in a form of minimum phase content, the XRD-amorphous phases can be quantified. However, such constraints are only valid for the cases studied and limit the general applicability and predictive power of the model. Elastic properties and strength of mortars are influenced by the metakaolin additions in an opposite trend. It indicates that they are sensitive to different microstructural features/mechanisms. Continuum micromechanic-based model is capable to accurately predict the performance evolution based on the volume of hydrates predicted by the thermodynamic modelling. An additional step required for the accurate prediction - porosity is partitioned based on its saturation at 95% RH – is introduced and substantiated.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Characterization of novel blast-furnace slag cement pastes and mortars activated with a reactive mixture of MgO-NaOH

This paper reports results of strength and reaction products of blast-furnace slag cements activated using a mixture of MgO-NaOH with a ratio 50/50 incorporated at 4, 6 and 8% relative to the slag mass. Pastes and mortars were prepared and cured at 20 °C and 60 °C-24 h-20 °C up to 90 days. The results indicated that the combination of MgO-NaOH acts as an effective alkaline activator of the slag, as samples cured at 20 °C developed 54 MPa at 90 days, while those at 60 °C-24 h-20 °C had a rapid strength gain at early ages but in the long run strengths of ~42 MPa at 90 days were observed. The microstructures consisted of (C-(A)-S-H), third aluminate hydrates and hydrotalcite. The formation of the latter increased at higher MgO:NaOH concentration lowering the Al uptake by C-S-H. MgO and Mg(OH){sub 2} were not detected, indicating an effective incorporation of Mg{sup 2+} ions into the atomic structure of the reaction products.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Influence of calcium and magnesium carbonates on hydration kinetics, hydrate assemblage and microstructural development of metakaolin containing composite cements

The hydration of metakaolin composite cements containing quartz, natural limestone and dolomite rock is studied using a multi-method approach and modelling. The study demonstrates that the calcite present in limestone and dolomite rock is very reactive. Contrary, dolomite does not dissolve. Additionally to the previously reported stabilization of ettringite, the reaction of calcite introduces several changes to the mechanism of metakaolin pozzolanic reaction. Namely, the silicate and aluminate distribution among the hydrates is different. In carbonate containing samples, experimental results supported by the thermodynamic modelling suggest that the silicate mainly precipitates as low Ca/Si C-S-H and additionally the ettringite content is higher. In the case of quartz analogue, the silicates precipitate as strätlingite and C-S-H of higher Ca/Si. These changes cause lower porosity as observed by SEM-BSE and higher strength. High metakaolin reactivity results in a very dense matrix that in turn enables co-existence of phases that are thermodynamically non-compatible.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Reactive transport modelling of cement paste leaching in brines

We propose and analyse a unified reactive transport model for leaching of cement paste in brines, with and without CO{sub 2}. We investigate the impact of the boundary conditions on the rate of propagation of the reaction. In agreement with experiments, we observe distinct mechanisms as a function of the pH and the CO{sub 2} concentration of the leaching brine. In particular, clogging is observed at intermediate concentration of CO{sub 2} while higher concentration accelerates the reaction. In addition, we leverage the flexibility of the simulator to explore the impact of different models on the simulations. In particular, aqueous species, phase assemblage and diffusion coefficient model are varied. We demonstrate that in order to be able to obtain quantitative predictions, it is important to accurately capture the feedback between chemical reactions, microstructure and macroscopic transport parameters.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Influence of fly ash and metakaolin on the microstructure and compressive strength of magnesium potassium phosphate cement paste

The influences of fly ash and metakaolin added as substitutions (by up to 50 wt%) of magnesium potassium phosphate cement (MKPC) on the microstructures and compressive strengths of the MKPC pastes were investigated. The results indicate that the aluminosilicate fractions of both fly ash and metakaolin are involved in the acid-base reaction of MKPC system, leading to a preferential formation of irregular crystalline struvite-K incorporated with Al and Si elements and/or amorphous aluminosilicate phosphate products. Metakaolin is more reactive than fly ash in the MKPC system. For the same addition dosage, the MKPC pastes containing metakaolin exhibit higher compressive strengths than the pastes containing fly ash. This is attributed to the formation of more highly reinforced microstructures and denser interfaces between the metakaolin particle and hydration products (e.g. struvite-K) in the MKPC paste containing metakaolin. Addition of 30 wt% metakaolin increases the compressive strengths of MKPC pastes at all test ages.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Reactive transport modelling of a cement backfill for radioactive waste disposal

Cementitious materials are included in many geological disposal facilities for radioactive wastes, including the UK candidate backfill material Nirex Reference Vault Backfill (NRVB). As part of an ongoing programme of work to assess NRVB performance, 1-D reactive-transport models have been constructed to simulate reaction with different illustrative groundwater compositions. Variant cases were also produced to explore the effect of model assumptions on the predicted behaviour of the backfill. Depending on groundwater composition, cement alteration pathways included: carbonation; external sulphate attack; chloride attack; the formation of magnesium-rich solids; and the precipitation of secondary aluminosilicate minerals. In general, the models suggest that the pore space in backfill associated with radioactive waste disposal systems is likely to become clogged (to some degree) over time close to backfill-rock interfaces resulting in a reduction in capacity for solute transport. However, the models do not include all relevant process couplings which is potentially, an area for further work.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

Water vapor sorption isotherms, pore structure, and moisture transport characteristics of alkali-activated and Portland cement-based binders

Moisture transport plays a key role in determining the different durability-related features of cementitious materials. In this paper, moisture sorption in a range of low-calcium (geopolymer-type) and calcium-rich alkali-activated binders are studied and compared with that of Portland cement-based binders. Through the analysis of water vapor sorption isotherms (WVSI) and mercury intrusion porosimetry (MIP) test results, two vastly different pore structures were observed. Fly ash-based geopolymer-type binders showed a very porous structure where a large volume of mesopores coexisted with a significant volume of macropores. Alkali-activated slag binders, however, had a very fine pore structure, with a relative lack of large macropores. The different pore structure of fly ash-based and slag-based binders led to amplification of pore blocking and cavitation in blended systems by the addition of slag. Analysis of the sorption kinetics showed the prominent effect of the presence of calcium in the matrix to reduce the permeability.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Impact of an SRA (hexylene glycol) on irreversible drying shrinkage and pore solution properties of cement pastes

Cementitious materials shrink when exposed to decreasing relative humidities, which may result in cracking. Shrinkage reducing admixtures (SRAs) can be used to reduce this drying shrinkage. Although many studies have shown that SRAs reduce the surface tension of the pore solution, the effects of SRAs on other pore solution properties and their relationship to drying shrinkage have been poorly characterized. In this work, we investigate the impact of an SRA (hexylene glycol) on the drying and re-humidification of a cement paste over an extended relative humidity range. The reduction in the first drying shrinkage by the SRA depends on relative humidity. The SRA also significantly reduces the irreversible drying shrinkage. We concluded that the SRA impacts drying shrinkage by acting on the capillary forces, by acting on the specific range of relative humidity over which those forces occur, and potentially by acting on the surface stresses through pore wall adsorption.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Robustness of cement-based materials: From dosage variations to yield stress fluctuations

The idea behind the present work is to assess robustness of fresh cement-based materials (i.e. their ability to display the same properties when submitted to variations in the way they are produced) from a generic and analytical point of view. First, analytical models from literature relating components proportions and yield stress are combined into a multi-scale and physical approach and compared to our experimental yield stress measurements. In the second part, the derivation of these analytical relationships is used to assess robustness as a function of components proportions, which allows for the most sensitive variations to be mapped onto component dosage from a yield stress point of view. In the case of fluid concretes, this approach showcases the interest of working at slightly higher water content and slightly lower aggregates fraction along with benefits of viscosity modifying agents / plasticizers combination.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Autogenous formation and smart behaviors of nitrite- and nitrate-intercalated layered double hydroxides (LDHs) in Portland cement-metakaolin-dolomite blends

In this work, the influence of sodium nitrite (NaNO{sub 2}) and sodium nitrate (NaNO{sub 3}) corrosion inhibitors on the composition, structure, and chloride binding behaviors of layered double hydroxides (LDHs) formed in ternary ordinary Portland cement-metakaolin-dolomite (OPC-MK-DM) systems is studied. The results show that the nitrite and nitrate anions are preferably intercalated in the CaAl LDHs (AFm phases), but not in the MgAl LDHs (hydrotalcite-type phases) due to its limited formation in these ternary cementitious systems cured at ambient temperature. The autogenously formed nitrate- and nitrite-AFm phases are decomposed upon chloride exposure accompanied by Friedel's salts formation, potentially releasing corrosion inhibitive ions to the pore solution in a progressive manner. The NaNO{sub 2} and NaNO{sub 3} incorporation in ternary OPC-MK-DM binders marginally lowers chloride binding capacity but reduces its penetration resistance mainly due to pore coarsening. Nevertheless, a strong linear correlation can be established between the water-soluble and total chloride contents in ternary OPC-MK-DM systems, regardless of OPC replacement level and corrosion inhibitor incorporation.

36 MATERIALS SCIENCE↗