How sulfates and increased temperature affect delayed ettringite formation (DEF) in white cement mortars

In this study,white cement CEM I and white limestone cement CEM II-LL A and Β with 15%, 25% and 35% limestone substitution were studied. The way delayed ettringite is forming due to exposure to increased temperature (50 °C) and external sulfate attack was examined in mortar samples which were immersed for 90 days in three different solutions: (a) saturated solution Ca(OH)₂ at 50 °C, (b) saturated solution of Ca(OH)₂ at 20 °C and (c) 5% w/w Na₂SO₄ solution at 50 °C. During this period mortar samples were visually observed regularly while their expansion was estimated on a weekly basis by measuring the change of length with a micrometer. At the end of the 90-days period the compressive strength of the mortars was determined and the deterioration products were identified through means of X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and thermogravimetric analysis (DTG). The results of this study show that DEF occurred in two forms. Samples cured at increased temperature contained DEF type I, which caused mediocre expansion and damage. Samples cured at increased temperature in the presence of sulfates produced DEF type II, which caused significant damage on the surface and exhibited high expansion.     

Performance of limestone cement mortars in a high sulfates environment

With the aim of studying the influence of cement composition on resistance in high sulfates environment, standard mortars have been produced using ordinary Portland cement (CEM I – 32.5) and limestone cement with 35% limestone (CEM II/B-LL – 32.5). The pore size distribution of the cement pastes was measured. The mortars were immersed in a 5% Na₂SO₄ solution at 20 °C for 1.5 years and the caused deterioration was been visually observed at a regular basis. Furthermore, the mortars expansion was being estimated by measuring the change of length. At the end of the experiment the compressive strength of the mortars was measured. The deterioration products of the mortars have been identified by means of X-ray diffraction, optical microscopy and environmental scanning electron microscopy. The limestone cement based mortar presented cracking that started at the age of 6 months and continued throughout the experiment. It also displayed high expansion after 250 days of immersion in a 5% Na₂SO₄ caused, as proved using the analytical techniques, by the formation of gypsum and ettringite. Concluding, the cement with 35% limestone did not perform as well as ordinary Portland cement under the most aggressive laboratory conditions. Hence, it is obvious that the addition of limestone in the cement leads to a totally different behaviour than Portland cement with respect to the resistance in high sulfates environment.     

Effects of limestone replacement ratio on the sulfate resistance of Portland limestone cement mortars exposed to extraordinary high sulfate concentrations

A comparative study has been performed on the sulfate resistance of Portland limestone cement (PLC) mortars exposed to extraordinary high sulfate concentrations (200 g/l). PLCs have been prepared by using two types of clinkers having different C₃S/C₂S ratios and interstitial phase morphologies. Blended cements have been prepared by replacing 5%, 10%, 20% and 40% of clinker with limestone. Cubic (50 × 50 × 50 mm) and prismatic (25 × 25 × 285 mm) cement mortars were prepared. After two months initial water curing, these samples were exposed to three different sulfate solutions (Na₂SO₄ at 20 °C and 5 °C, MgSO₄ at 5 °C). Solutions were not refreshed and pH values of solutions were monitored during the testing stage. The compressive strength and length changes of samples have been monitored for a period of 1 year. Additional microstructural analyses have been conducted by XRD and SEM/EDS studies. Results indicated that in general, limestone replacement ratio and low temperature negatively affect the sulfate resistance of cement mortars. Additionally, clinkers of high C₃S/C₂S ratios with dendritic interstitial phase structure were found to be more prone to sulfate attack in the presence of high amounts of limestone.From the results, it is postulated that in the absence of solution change, extraordinary high sulfate content modified the mechanism of sulfate reactions and formation of related products. At high limestone replacement ratios, XRD and SEM/EDS studies revealed that while ettringite is the main deterioration product for the samples exposed to Na₂SO₄, gypsum and thaumasite formation were dominant products of deterioration in the case of MgSO₄ attack. It can be concluded that, the difference between reaction mechanisms of Na₂SO₄ and MgSO₄ attack to limestone cement mortars strongly depends on the pH change of sulfate solutions.     

Thaumasite form of sulfate attack in limestone cement mortars: A study on long term efficiency of mineral admixtures

Concrete and mortar made from limestone cement may exhibit a lack of durability due to the formation of thaumasite. The addition of minerals that improve the concrete durability is expected to slow down the formation of thaumasite. In this work the effect of natural pozzolana, fly ash, ground granulated blastfurnace slag and metakaolin on the thaumasite formation in limestone cement mortar is examined. A limestone cement, containing 15% w/w limestone, was used. Mortar specimens were prepared by replacing a part of limestone cement with the above minerals. The specimens were immersed in a 1.8% MgSO₄ solution and cured at 5 and 25 °C. The status of the samples after a storage period of 5 years was reported based on visual inspection, compressive strength, mass measurements, ultrasonic pulse velocity measurements and analytical techniques. It is concluded that the use of specific minerals, as partial replacement of cement, inhibits thaumasite formation in limestone cement mortar.     

Performance of self-compacting concrete containing different mineral admixtures

This paper presents experimental study on the properties of self-compacting concrete (SCC). Portland cement (PC) was replaced with fly ash (FA), granulated blast furnace slag (GBFS), limestone powder (LP), basalt powder (BP) and marble powder (MP) in various proportioning rates. The influence of mineral admixtures on the workability, compressive strength, ultrasonic pulse velocity, density and sulphate resistance of SCC was investigated. Sulphate resistance tests involved immersion in 10% magnesium sulphate and 10% sodium sulphate solutions for a period of 400 days. The degree of sulphate attack was evaluated using visual examination and reduction in compressive strength. The test results showed that among the mineral admixtures used, FA and GBFS significantly increased the workability and compressive strength of SCC mixtures. Replacing 25% of PC with FA resulted in a strength of more than 105 MPa at 400 days. Moreover, the presence of mineral admixtures had a beneficial effect on the strength loss due to sodium and magnesium sulphate attack. On the other hand, the best resistance to sodium and magnesium sulphate attacks was obtained from a combination of 40% GBFS with 60% PC.     

Microstructure changes in mortars attacked by sulphates at 5 °C

In this study mortars have been produced using ordinary Portland cement (CEM I – 32.5) and limestone cement with 15% limestone addition (CEM II/A-LL – 32.5). The mortars were immersed in a solution of 5% Na₂SO₄ at 5 °C for 6 months and the caused deterioration was observed visually at a regular basis. The deterioration product of the surface of both mortars has been identified as thaumasite by the means of XRD, FT-IR, DTA and SEM/EDAX analysis. The damage caused due to formation of thaumasite in both mortars was approximately the same and not influenced by the addition of limestone. Furthermore, expansion and compressive strength of the mortars were studied as a function of time and it was proved they were not influenced by thaumasite formation at the age of 6 months.     

Filler effect and pozzolanic reaction of ground palm oil fuel ash

This research examines the compressive strength of mortar and how the filler effect and pozzolanic reaction of ground palm oil fuel ash (POFA) contribute to this strength. POFA and river sand were ground to three different particle sizes and used to replace Type I Portland cement at 10–40% by weight of binder to cast the mortar. The compressive strengths of ground POFA and ground river sand mortars were determined at various ages between 7 and 90 days. The results showed that the compressive strength of mortar due to the filler effect of ground river sand was nearly constant during the 7–90 day period for a specified replacement rate of cement. However, the compressive strength of mortar due to the filler effect tended to increase slightly with increased cement replacement. The pozzolanic reaction of ground POFA increased with increasing particle fineness of ground POFA, replacement rate of cement, and age of the mortar. The compressive strength contribution from the pozzolanic reaction of ground POFA was much more pronounced than the contribution from the filler effect when the smallest sizes of both materials were considered.     

High strength characteristics of cement mortar reinforced with hybrid fibres

An experimental study was conducted on high strength mortar reinforced with steel fibres and hybrid fibres consisting of steel fibre, palm fibre and synthetic fibre (Barchip). The inclusion of fibres was maintained at a volumetric fraction of 2%. The compressive strength, splitting tensile strength, static modulus of elasticity, shrinkage, flexural strength, and flexural toughness were determined to study the effect of the hybrid fibres on the properties of high strength cement mortar (HSCM). The results showed that hybridization of fibres in the quantities 1.5% steel fibres + 0.25% palm fibres + 0.25% Barchip fibres, improved the compressive strength and flexural toughness significantly, and also enhanced the splitting tensile strength and flexural strength of the mortar by about 44% and 140%, respectively.     

Utilization of separator bag filter dust for high early strength cement production

This paper presents the feasibility of incorporating ultra-fine particles collected in the separator bag filter during the process of manufacturing cement (SBFC) as an substitution material for cement. Approximately 2.5% of SBFC is produced during OPC manufacturing process. Also, the average size of SBFC particles is about 5 μm, the average size of OPC particles is about 14 μm. This method does not require additional processes needed in the existing processes to manufacture high early strength cement such as modifying mineral components and adjusting the firing temperature. Moreover, it can also solve the issue of efficiency decrease resulted from the increase of the grinding time applied in the existing process of manufacturing microcement. In order to investigate the characteristic properties of this cement mixture, cement blends have been produced by using different amounts of SBFC. While the blaine value of 100% SBFC was significantly higher (6953 cm²/g) than that of Ordinary Portland Cement (OPC), its chemical composition showed no significant difference. Cement paste, mortar mixtures have been prepared by using cement blends incorporating 0, 50 and 100% SBFC by weight. Flowability, setting time and compressive strength tests has been performed. Test results showed that substitution of SBFC negatively affect the flowability of cement paste and mortar mixtures. Moreover, setting times shortened, compressive and flexural strength values increased by the substitution of SBFC. Finally, microstructure analysis of cement paste samples showed that incorporation of SBFC reduced the internal porosity by 9% as determined by the proposed method. The internal porosity of paste was measured by mercury intrusion porosimetry (MIP). The compressive strength and bending strength of mortar were higher in the order of 100, 50 and 0% SBFC mixed.     

Development of alpha plaster from phosphogypsum for cementitious binders

Efforts have been made to make high strength alpha plaster from phosphogypsum, a by-product of phosphoric acid industry. Phosphogypsum was autoclaved in slurry form (phosphogypsum 50% + water 50%, by wt.) in the laboratory at different steam pressures for different durations in presence of chemical admixtures. It was found that with small quantity of chemical admixture (sodium succinate/potassium citrate/sodium sulphate), alpha plaster of high strength can be produced. The optimum pressure and duration of autoclaving was found to be as 35 psi and 2.0 h, respectively. The alpha plaster was examined for making cementitious binders by admixing hydrated lime, fly ash, granulated blast furnace slag, marble dust and chemical additives with alpha plaster. Data showed that cementitious binder of compressive strength of 22.0 and 30 MPa (at 28 days of curing at 40° and 50 °C) and low water absorption was produced. DTA and SEM studies of the binder showed formation of CSH, ettringite and C₄AH₁₃ as main cementitious products to give strength.     

Hybrid effect of carbon nanotube and nano-clay on physico-mechanical properties of cement mortar

In this work, several nanomaterials have been used in cementitious matrices: multi wall carbon nanotubes (MWCNTs) and nano-clays. The physico-mechanical behavior of these nanomaterials and ordinary Portland cement (OPC) was studied. The nano-clay used in this investigation was nano-kaolin. The metakaolin was prepared by thermal activation of nano-kaolin clay at 750 °C for 2 h. The organic ammonium chloride was used to aid in the exfoliation of the clay platelets. The blended cement used in this investigation consists of ordinary Portland cement, carbon nanotubes and exfoliated nano metakaolin. The OPC was substituted by 6 wt.% of cement by nano metakaolin (NMK) and the carbon nanotube was added by ratios of 0.005, 0.02, 0.05 and 0.1 wt.% of cement. The blended cement: sand ratio used in this investigation was 1:2 wt.%. The blended cement mortar was prepared using water/binder ratio of 0.5 wt.% of cement. The fresh mortar pastes were first cured at 100% relative humidity for 24 h and then cured in water for 28 days. Compressive strength, phase composition and microstructure of blended cement were investigated. The results showed that, the replacement of OPC by 6 wt.% NMK increases the compressive strength of blended mortar by 18% compared to control mix and the combination of 6 wt.% NMK and 0.02 wt.% CNTs increased the compressive strength by 29% than control.     

Freeze–thaw resistance of blended cements containing calcined paper sludge

This work deals with the frost resistance of blended cements containing calcined paper sludge (source for metakaolin) as partial Portland cement replacements. Freeze–thaw tests were performed on blended cement mortars containing 0%, 10% and 20% waste paper sludge calcined at 650 °C for 2 h. Cement mortar specimens were exposed to freezing and thawing cycles until the relative dynamic modulus of elasticity fell below 60%. The performance of the cement mortars was assessed from measurements of weight, ultrasonic pulse velocity, compressive strength, mercury intrusion porosimetry and SEM. Failure of the control cement mortar occurred before 40 freeze/thaw cycles, while cement mortar containing 20% calcined paper sludge failed after 100 cycles. After 28 and 62 freezing and thawing cycles, cement blended with 10% and 20% calcined paper sludge exhibited a smaller reduction in compressive strength than the control cement.     

Evaluation of sulfate resistance of Portland and high alumina cement mortars using hardness test

Portland cement and high alumina cement mortar specimens were exposed to cycles of drying at 40 °C, cooling at 20 °C and immersion in Na₂SO₄ and MgSO₄ solutions at 20 °C. The resistance of mortars was evaluated by visual inspection and by measuring the change in surface hardness and weight of the specimens. The decrease and increase in surface hardness were observed in both mortars by treating with Na₂SO₄ and MgSO₄ solutions, respectively. The combined effect of the chemical and physical attack by Na₂SO₄ was attributed to the complete failure of Portland cement mortar, whereas only marginal damage of high alumina cement mortar was believed owing to physical salt crystallization. No damage was observed in both mortars treated with MgSO₄ solution.     

Early hydration of calcium sulfoaluminate cement through electrical resistivity measurement and microstructure investigations

The electrical resistivities of the calcium sulfoaluminate (CSA) cement pastes at different water to cement (W/C) ratios, over a period of 1440 min (or 24 h) were measured by a non-contacting electrical resistivity apparatus. The electrical resistivity–time curve decreased slightly after mixing, and then increased sharply around the setting time, followed by two peaks, and finally developed at a very low rate up to 1440 min. The porosity plays a dominant role in the electrical resistivity development of the CSA cement paste in the earlier period of hydration (before the initial setting time), while the ion concentration plays a major role at the later period (after the second peak). The electrical resistivity–time curve demonstrates the process of ettringite formation and transformation to monosulfate in the CSA hydration system, and this is confirmed by the SEM and XRD observations. The high temperature and the insufficiency of gypsum in the CSA cement system during hydration result in the decomposition of ettringite at the first peak, while at the second peak the decomposition of ettringite is due to the lack of gypsum. The relationship between W/C and electrical resistivity at 1 h follows a negative trend but a positive trend is observed at 24 h. The relationship between the compressive strength and the electrical resistivity at 24 h for the different W/C ratios follows a negative relationship.     

Influence of activator on the strength and drying shrinkage of alkali-activated slag mortar

The development of new binders, as an alternative to traditional cement, by the alkaline activation of industrial by-products (i.e. ground granulated slag and fly ash) is an ongoing research topic in the scientific community [Puertas F, Amat T, Jimenez AF, Vazquez T. Mechanical and durable behaviour of alkaline cement mortars reinforced with polypropylene fibres. Cem Concr Res 2003;33(12): 2031–6]. The aim of this study was to investigate the feasibility of using and alkaline activated ground Turkish slag to produce a mortar without Portland cement (PC).Following the characterization of the slag, mortar specimens made with alkali-activated slag were prepared. Three different activators were used: liquid sodium silicate (LSS), sodium hydroxide (SH) and sodium carbonate (SC) at different sodium concentrations. Compressive and flexural tensile strength of alkali-activated slag mortar was measured at 7-days, 28-days and 3-months. Drying shrinkage of the mortar was measured up to 6-months. Setting times of the alkali-activated slag paste and PC paste were also measured.Setting times of LSS and SH activated slag pastes were found to be much slower than the setting time of PC paste. However, slag paste activated with SC showed similar setting properties to PC paste.LSS, SH and SC activated slag mortar developed 81, 29, and 36 MPa maximum compressive strengths, and 6.8, 3.8, and 5.3 MPa maximum flexural tensile strengths at 28-days. PC mortar developed 33 MPa compressive strength and 5.2 MPa flexural tensile strength. LSS and SH activated slag mortars were found to be more brittle than SC activated slag and PC mortars.Slag mortar made with LSS had a high drying shrinkage, up to six times that of PC mortar. Similarly, slag mortar made with SH had a shrinkage up to three times that of PC mortar. However, SC activated slag mortar had a lower or comparable shrinkage to PC mortar. Therefore, the use of SC as an activator for slag mortar is recommended, since it results in adequate strength, similar setting times to PC mortar and comparable or lower shrinkage.     

Effects of curing regimes and cement fineness on the compressive strength of ordinary Portland cement mortars

Curing techniques and curing duration have crucial effects on the strength and other mechanical properties of mortars. Proper curing can protect against moisture loss from fresh mixes. The objective of this experimental work is to examine the compressive strength of ordinary Portland cement mortars (OMs) under various curing regimes and cement fineness. Six different curing methods including water, air, water heated, oven heated, air–water, and water–air were applied to the specimens and also six groups of mortars were used. The results showed that the highest and lowest compressive strengths are attributed to the specimens of OPC mortar water cured using grounded OPC for duration of 6 h (OM–G6–wc) and OPC mortar air cured under room temperature with oven heated after demoulding of the specimens at 60 °C for duration of 20 h (OM–OH–ac), respectively. The maximum levels obtained of compressive strengths at 7, 28, and 90 days are 57.5, 70.3, and 76.0 MPa, respectively.     

Increasing mortar strength with the use of activated kaolin by-products from paper industry

Making use of industrial by-product or waste clay to partially replace cement in concrete has greatly contributed to sustainable development of environment. This study investigated the optimal activation condition for producing high reactivity metakaolin (MK) by using kaolin by-products (KB) from paper industry. Initially, the material properties of KB were analyzed in this study and the results indicated its great potential to be treated by calcination to be a very effective pozzolan. Afterwards, MK samples produced from different activation treatments of KB, including different calcining temperature, calcining duration, initial temperature rise rime and grinding particle size, were applied in mortar to determine their pozzolanic effect. Results indicated that the optimal activation condition for KB to high reactivity MK conversion is 2-h calcining duration at 750 °C and with 7 μm grinding particle size. Finally, compressive and flexural strengths of mortar samples produced by replacing cement with 0–25% MK content were tested and the results showed that 15% was the optimal cement replacement level of MK and the mortar so produced exhibited 20% improvement in compressive strength compared to control mortar.     

Sulphate resistance of fibre reinforced cement-based foams

This paper describes the results of an investigation on the resistance of plain and fibre reinforced cement-based foams to sulphate exposure. A synthetic foaming agent was used to produce foamed cementitious composites with essentially a closed cellular structure at 1200 kg/m³, 750 kg/m³, and 475 kg/m³. Polymeric microfibres were introduced at 0% and 0.2% volume fraction to result in 6 mixes. Prismatic specimens were immersed in a sodium sulphate solution to be tested in flexure, after specific intervals of exposure, according to ASTM C1609. A comparison with the response of unexposed specimens reveals that the heavier cement-based foams are more susceptible to sulphate attack and perform poorly with an increase in the duration of exposure. On the other hand, the lightest of the mixes—at 475 kg/m³—registered higher flexural strength and toughness factors up to 30 days of exposure before succumbing to sulphate attack. This self-healing response was attributed to the space available in such highly porous composites that allows for the unhindered growth of ettringite without attendant cracking. The presence of microfibres facilitated self-healing, as evident from the flexural toughness factor.     

Use of natural and thermally activated porphyrite in cement production

The aim of the present study was to investigate the use of porphyrite in the production of Portland cement. Natural and thermally activated porphyrites were used as a clay raw material and an activator, respectively, at 0, 10, 20, 30, 40 and 50 wt% in order to assess their effects on the cement properties. According to the test results, the compressive strength of the specimens decreased with increasing natural porphyrite content in various curing periods. However, the compressive strength of cement produced with 10 wt% porphyrite (activator) activated at 650 °C for 30 min showed a higher value (56 MPa in TPC-6) than cement without activator (51 MPa in RPC-2). Due to thermal activation, porphyrite activator containing a glass phase possesses an enhanced reactivity during clinker hydration that intensifies the synthesis of hydrosilicates and improves compressive strength accordingly. The X-ray diffraction analysis confirmed an intensive formation of Portland cement minerals such as C₃S, β-C₂S, C₃A and C₄AF. The addition of thermally activated porphyrite has also led to an improvement of the rheological behavior, stability to expansion, increase in setting time and decrease in specific surface area of cement. As prepared cement composites and concretes with improved properties meet the requirements of State Standards 310-86 and 10181-81 for Portland cement and concrete, respectively. The findings in this report indicate that porphyrite can be utilized both as a raw material and an activator in the production of cement.     

Influence of calcined kaolin on mortar properties

The use of calcined clay, in the form of metakaolin (MK), as a pozzolanic material for mortar and concrete has received considerable attention in recent years. The present paper describes the results of a research project initiated to study the calcination of local kaolin at various temperatures (650–950 °C) and durations (2, 3 and 4 h) to produce MK with a high pozzolanic activity. The pozzolanic activity was assessed by 28-days compressive strength and hydration heat methods. The maximum identified activity was obtained at 850 °C for 3 h duration. An increase of both hydration heat and compressive strength was obtained when ordinary Portland cement was replaced by 10% MK. The use of ternary blended cement improves the early age and the long-term compressive strength. The durability was also enhanced as better acidic resistance was observed.