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At least 1,423 records · Page 79
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DOE OSTI2014

Amorphous silica in ultra-high performance concrete: First hour of hydration

Amorphous silica in the sub-micrometer size range is widely used to accelerate cement hydration. Investigations including properties of silica which differ from the specific surface area are rare. In this study, the reactivity of varying types of silica was evaluated based on their specific surface area, surface silanol group density, content of silanol groups and solubility in an alkaline suspension. Pyrogenic silica, silica fume and silica synthesized by hydrolysis and condensation of alkoxy silanes, so-called Stoeber particles, were employed. Influences of the silica within the first hour were further examined in pastes with water/cement ratios of 0.23 using in-situ X-ray diffraction, cryo scanning electron microscopy and pore solution analysis. It was shown that Stoeber particles change the composition of the pore solution. Na{sup +}, K{sup +}, Ca{sup 2+} and silicate ions seem to react to oligomers. The extent of this reaction might be highest for Stoeber particles due to their high reactivity.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Characterization of morphology and hydration products of high-volume fly ash paste by monochromatic scanning x-ray micro-diffraction (μ-SXRD)

The present study focuses on identification and micro-structural characterization of the hydration products formed in high-volume fly ash (HVFA)/portland cement (PC) systems using monochromatic scanning x-ray micro-diffraction (μ-SXRD) and SEM-EDS. Pastes with up to 80% fly ash replacement were studied. Phase maps for HVFA samples using μ-SXRD patterns prove that μ-SXRD is an effective method to identify and visualize the distribution of phases in the matrix. μ-SXRD and SEM-EDS analysis shows that the C-S-H formed in HVFA system containing 50% or more of fly ash has a similar structure as C-S-H(I) with comparatively lower Ca/Si ratio than the one produced in PC system. Moreover, coexistence of C-S-H(I) and strätlingite is observed in the system containing 80% of fly ash, confirming that the amount of alumina and silicate phases provided by the fly ash is a major factor for the formation of C-S-H(I) and strätlingite in HVFA system. - Highlights: • High-volume fly ash (HVFA) paste was studied by scanning x-ray micro-diffraction. • Coexistence of C-S-H(I) and strätlingite in the HVFA system is clearly shown. • The distribution of minor phases in the HVFA system is shown. • Differences between inner and outer products of fly ash are observed by SEM-EDS.

36 MATERIALS SCIENCE↗
DOE OSTI2014

XPS characterization of polymer–monocalcium aluminate interface

The aim of this paper is the introduction of a sophisticated testing method, X-ray photoelectron spectroscopy (XPS), used to study the interface between the hydrated cement phase and polymer after mechanochemical activation, which is fundamental for the creation of macro-defect-free (MDF) composites. The XPS results clearly explain the hypothesis of a chemical reaction mechanism in the interphase regions affecting the final properties of the MDF materials.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Effect of temperature and aluminium on calcium (alumino)silicate hydrate chemistry under equilibrium conditions

There exists limited information regarding the effect of temperature on the structure and solubility of calcium aluminosilicate hydrate (C–A–S–H). Here, calcium (alumino)silicate hydrate (C–(A–)S–H) is synthesised at Ca/Si = 1, Al/Si ≤ 0.15 and equilibrated at 7–80 °C. These systems increase in phase-purity, long-range order, and degree of polymerisation of C–(A–)S–H chains at higher temperatures; the most highly polymerised, crystalline and cross-linked C–(A–)S–H product is formed at Al/Si = 0.1 and 80 °C. Solubility products for C–(A–)S–H were calculated via determination of the solid-phase compositions and measurements of the concentrations of dissolved species in contact with the solid products, and show that the solubilities of C–(A–)S–H change slightly, within the experimental uncertainty, as a function of Al/Si ratio and temperature between 7 °C and 80 °C. These results are important in the development of thermodynamic models for C–(A–)S–H to enable accurate thermodynamic modelling of cement-based materials.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Electrical resistance tomography to monitor unsaturated moisture flow in cementitious materials

Traditionally the electrically-based assessment of the moisture flow in cement-based materials relies on two- or four-point measurements. In this paper, imaging of moisture distribution with electrical resistance tomography (ERT) is considered. Especially, the aim is to study whether ERT could give information on unsaturated moisture flows in cases where the flow is non-uniform. In the experiment, the specimens are monitored with ERT during the water ingress. The ERT reconstructions are compared with neutron radiographs, which provide high resolution information on the 2D distribution of the moisture. The results indicate that ERT is able to detect the moisture movement and to show approximately the shape and position of the water front even if the flow is nonuniform.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Identification of the hydrate gel phases present in phosphate-modified calcium aluminate binders

The conversion of hexagonal calcium aluminate hydrates to cubic phases in hydrated calcium aluminate cements (CAC) can involve undesirable porosity changes and loss of strength. Modification of CAC by phosphate addition avoids conversion, by altering the nature of the reaction products, yielding a stable amorphous gel instead of the usual crystalline hydrate products. Here, details of the environments of aluminium and phosphorus in this gel were elucidated using solid-state NMR and complementary techniques. Aluminium is identified in both octahedral and tetrahedral coordination states, and phosphorus is present in hydrous environments with varying, but mostly low, degrees of crosslinking. A {sup 31}P/{sup 27}Al rotational echo adiabatic passage double resonance (REAPDOR) experiment showed the existence of aluminium–phosphorus interactions, confirming the formation of a hydrated calcium aluminophosphate gel as a key component of the binding phase. This resolves previous disagreements in the literature regarding the nature of the disordered products forming in this system.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Plastic shrinkage of mortars with shrinkage reducing admixture and lightweight aggregates studied by neutron tomography

Water transport in fresh, highly permeable concrete and rapid water evaporation from the concrete surface during the first few hours after placement are the key parameters influencing plastic shrinkage cracking. In this work, neutron tomography was used to determine both the water loss from the concrete surface due to evaporation and the redistribution of fluid that occurs in fresh mortars exposed to external drying. In addition to the reference mortar with a water to cement ratio (w/c) of 0.30, a mortar with the addition of pre-wetted lightweight aggregates (LWA) and a mortar with a shrinkage reducing admixture (SRA) were tested. The addition of SRA reduced the evaporation rate from the mortar at the initial stages of drying and reduced the total water loss. The pre-wetted LWA released a large part of the absorbed water as a consequence of capillary pressure developing in the fresh mortar due to evaporation.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Effects of temperature on the atomic structure of synthetic calcium–silicate–deuterate gels: A neutron pair distribution function investigation

Due to the nanocrystallinity of the calcium–silicate–hydrate (C–S–H) gel in ordinary Portland cement-based paste combined with the presence of nanoscale heterogeneities such as varying calcium-to-silicon ratios and incorporation of aluminum in the structure, standard characterization techniques fail to fully capture the complex atomic structure and nanoscale morphology of this important binder phase. Here, neutron pair distribution function (PDF) analysis is applied to a range of deuterated C–S–H gels with varying Ca/Si ratios (denoted C–S–D). In situ temperature measurements reveal that the local atomic bonding environments in C–S–D gel undergo large structural rearrangements due to exposure to elevated temperature (above ~ 200 °C), including the collapse of the C–S–D gel interlayer spacing to 9.6 Å and the emergence of a disordered dicalcium silicate phase (similar to larnite). At lower elevated temperatures, the atom–atom correlations are dominated by scattering from deuterium atoms and therefore can be used to quantify the dehydration kinetics.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Chloride-induced corrosion mechanism and rate of enamel- and epoxy-coated deformed steel bars embedded in mortar

The chloride-induced corrosion mechanisms of uncoated, pure enamel (PE)-coated, mixed enamel (ME)-coated, double enamel (DE)-coated, and fusion bonded epoxy (FBE)-coated deformed steel bars embedded in mortar cylinders are investigated in 3.5 wt.% NaCl solution and compared through electrochemical tests and visual inspection. Corrosion initiated after 29 or 61 days of tests in all uncoated and enamel-coated steel bars, and after 244 days of tests in some FBE-coated steel bars. In active stage, DE- and FBE-coated steel bars are subjected to the highest and lowest corrosion rates, respectively. The uncoated and ME-coated steel bars revealed relatively uniform corrosion while the PE-, DE-, and FBE-coated steel bars experienced pitting corrosion around damaged coating areas. Due to the combined effect of ion diffusion and capillary suction, wet–dry cyclic immersion caused more severe corrosion than continuous immersion. Both exposure conditions affected the corrosion rate more significantly than the water–cement ratio in mortar design.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Link between microstructure and tritiated water diffusivity in mortars: Impact of aggregates

The present study aims to investigate the influence of microstructure, particularly the effect of aggregates content and interfacial transition zone (ITZ), on tritiated water (HTO) diffusivity in mortars. To this end, three different series of mortars were prepared and HTO diffusion tests were conducted. Variables are water-to-cement ratio, sand volume fractions, and particle size distribution. In parallel, the microstructure of these materials was characterized by water porosimetry, mercury porosimetry, and by backscattered electron microscopy associated to images analysis. It was observed that at low sand content (0%–50%), diffusion properties of mortars are dominated by aggregates dilution effect. Beyond 50% of standard sand, other effects related to the large number of sand grains appear, such as air voids and porous areas mainly due to the difficulty of obtaining well-compacted materials.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Synthesis of monocrystalline Ca{sub 3}SiO{sub 5} using the optical floating zone method

Alite (Ca{sub 3}SiO{sub 5}/C{sub 3}S with low concentrations of foreign ions) is the main constituent of Ordinary Portland Cement. Normally it forms during sintering but with quite low crystal sizes (ca. 30 μm). For experiments on alite hydration behavior monocrystalline grains are required. Due to its incongruent melting behavior and its thermodynamic instability below 1250 °C it is very challenging to obtain large alite single crystals. In the present study, the floating zone method was used for annealing polycrystalline rods of monoclinic and triclinic C{sub 3}S just below the melting point of the phase. Large monocrystalline grains (> 500 μm) of the monoclinic (Al, Mg-doped) and triclinic polymorphs could successfully be obtained. Monocrystallinity was demonstrated by electron backscatter diffraction (EBSD). The chemical composition regarding incorporation of foreign ions and thus the resulting crystallographic modification of the C{sub 3}S can easily be adjusted. Chemical homogeneity of the synthesized monocrystalline grains was proven by electron probe microanalysis (EPMA).

36 MATERIALS SCIENCE↗
DOE OSTI2018

Earth concrete. Stabilization revisited

Not surprisingly, with the increased awareness of environmental issues, construction with raw (crude, unbaked) earth (subsoil) is gaining renewed interest. However, it suffers from a poor image and from the difficulty to meet modern productivity standards and to pass some durability tests designed for industrial materials. The recent trend is to overcome these drawbacks by “stabilizing” the material most often with Portland cement (PC). Here we show that stabilization with PC is in general neither technically nor environmentally advisable. It brings only moderate mechanical improvement at a high environmental cost. Rather than massively transforming crude earth into a low quality concrete, it would be more appropriate to adapt the architectural practice and/or to look for milder ways to improve properties. In this respect, the recent successful attempts to improve the workability and the strength of raw earth by controlling the dispersion of its fine fraction seem to be particularly promising.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Influence of freeze-thaw cycles on capillary absorption and chloride penetration into concrete

Combined mechanical and environmental actions reduce service life of reinforced concrete structures more than each of the participating actions alone. In this contribution, the influence of freeze-thaw cycles on capillary water absorption and chloride penetration into ordinary concrete with two different water-cement ratios and air-entrained concrete was investigated. Water profiles in concrete were quantified by neutron radiography. Capillary water absorption and chloride penetration are both slowed down considerably by air entrainment. Chloride ions dissolved in water are filtered out of the penetrating salt solution and remain concentrated near the surface. Capillary water absorption and chloride penetration into ordinary concrete are accelerated considerably by frost damage. After exposure to freeze-thaw cycles a damage gradient from the surface to the center of the samples was observed. Transport mechanisms were studied in some detail and the data obtained can serve as a basis for more realistic prediction of service life of reinforced concrete structures under the influence of combined freeze-thaw cycles and chloride penetration.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Development of MgO concrete with enhanced hydration and carbonation mechanisms

This study proposed the use of hydration agent (HA) and seeds to improve the hydration and carbonation of reactive magnesium cement (RMC)-based concrete formulations. Hydration of RMC was evaluated by isothermal calorimetry. Water absorption and compressive strength results were used to assess the mechanical performance of RMC-based concrete samples. Quantification of hydrate and carbonate phases was performed via XRD and TGA. Formation and morphology of carbonates were observed via BSE and SEM. In addition to increasing the utilization of RMC in the carbonation reaction and facilitating early strength development, the use of HA formed large carbonate phases, while the addition of seeds improved sample microstructures via the development of dense carbonate networks. The improvements in morphology, microstructure and carbonate content in samples involving the simultaneous use of HA and seeds resulted in 56% lower water absorption values and 46% higher 28-day compressive strengths (70 MPa) in comparison to the control sample.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Can calcium aluminates activate ternesite hydration?

Aluminum hydroxide (AH{sub 3}) has recently been shown to be able to activate hydration in ternesite, a phase found in some calcium sulfoaluminate (CSA) cements. This study explored the capacity of a number of calcium aluminates (C{sub 3}A, C{sub 12}A{sub 7}, CA and C{sub 4}A{sub 3} S-bar ) to activate ternesite hydraulic reactivity. After laboratory synthesis, the aluminates were blended with ternesite at a ratio of 1:2 and their hydration was monitored with isothermal conduction calorimetry for 7 days at 25 °C. The resulting pastes were analysed with XRD, FTIR and DTA. The presence of ternesite in the pastes altered the aluminate heat flow curves, shortening the induction period and bringing the reaction peak forward, an indication of hastened hydration. Ternesite also altered the reaction products, which included calcium monosulfoaluminate hydrate and strätlingite.

36 MATERIALS SCIENCE↗
DOE OSTI2018

A novel method to predict internal relative humidity in cementitious materials by 1H NMR

In sealed cementitious materials, the internal relative humidity (RH) decrease is mainly due to the water activity depression caused by menisci formation in partially-saturated pores. This process can be conveniently described with the evolution of the Kelvin radius. To obtain the Kelvin radius, a novel method based on the evolution of pore volumes quantified by {sup 1}H nuclear magnetic resonance (NMR) and mercury intrusion porosimetry (MIP) was developed. This approach was validated against experimental results for cementitious materials with a range of water to cement ratios from 0.30 to 0.46. A comparison between the Kelvin radius calculated with this approach with a previously published method using data obtained from MIP and chemical shrinkage was presented. A sensitivity analysis for the new prediction method was performed using a bootstrapping technique.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Determination of the amount of reacted metakaolin in calcined clay blends

This paper presents a comparative study of three methods to determine the amount of reacted metakaolin in calcined clay blends: mass balance, thermodynamic modelling, and the Partial or not Known Crystalline Structure method (PONKCS) based on Rietveld analysis of X-ray diffraction. The methods are applied to Limestone calcined clay cements (LC{sup 3}-50) in this study. Mass balance and thermodynamic modelling results show good agreement, especially at early age. PONKCS method shows globally comparable results, even if it has higher variability. The precision of PONKCS becomes poor for blends with <60% of metakaolin in calcined clay.

36 MATERIALS SCIENCE↗
DOE OSTI2018

A TEM study on the very early crystallization of C-S-H in the presence of polycarboxylate superplasticizers: Transformation from initial C-S-H globules to nanofoils

Polycarboxylate superplasticizers (PCEs) present common admixtures to adjust the rheology of concrete. Previous studies revealed that they can also influence the crystallization of cement hydrates, such as e.g. ettringite. In this study, we investigated the impact of methacrylate ester-based PCEs on the nucleation and crystal growth of C-S-H precipitated from aqueous solutions of Ca(NO{sub 3}){sub 2} and Na{sub 2}SiO{sub 3}. TEM imaging revealed that in the absence of PCEs following a non-classical nucleation mechanism C-S-H initially precipitates as metastable, globular nanoparticles (droplets, d ~ 20–60 nm) which within less than one hour convert to the characteristic nanofoils of early C-S-H. In the presence of PCEs, the initial globuli exhibit a core-shell morphology, presumably with PCE as shell. The shell was found to delay the conversion to nanofoils for several hours by stabilizing the metastable globules. The PCE polymer exhibiting higher anionicity delayed the conversion to nanofoils more than the PCE possessing fewer carboxylate groups.

36 MATERIALS SCIENCE↗