Effect of elevated temperature on alkali-activated geopolymeric binders compared to portland cement-based binders

This research focused on developing thermally-stable materials based on alkali-activation of slag, fly ash, and metakaolin compared to portland cement mixtures by using a hierarchical approach to material design. At lower length scales, X-ray diffraction (XRD) characterized the mineralogy that coupled to higher length scale experiments using thermogravimetric analysis (TGA) for determining the materials thermal stability. Additionally, high-energy X-ray computed microtomography (μCT) determined the best-performing material formulation that minimized thermal damage when exposed to high temperatures (650 °C). The thermal loading was ramped up to 650 °C from ambient temperature in 60 s and then held for a total of 10 min. The μCT identified that the alkali-activated fly ash mortar had less initial porosity than the ordinary portland cement mixtures, with more than 66% of the pores between 20 and 50 μm in diameter. Consequently, the alkali-activated fly ash mortar was able to dissipate approximately 565 °C in just 50 mm of material, outperforming all the other mixes studied in this paper with μCT confirming minimal damage after the temperature exposure.     

Recycling of harmful waste lead-zinc mine tailings and fly ash for preparation of inorganic porous ceramics

The porous ceramics were prepared by directly sintering of lead-zinc mine tailings and fly ash as the raw materials without any additional sintering and foaming agent. The effects of fly ash addition on the crystalline phases, pore structure, physical–chemical porosities and mechanical strength were investigated. The results showed that the bulk density decreased firstly and then increased while the porosity and water absorption presented the opposite tendency with the increase of fly ash content. Meanwhile, the chemical stability improved and the flexural strength had the same variation tendency of the bulk density. The phase evolution of sample with 60 wt% fly ash addition indicated that anorthite phase was formed at low temperature (1000 °C). The thermal behavior illustrated that the foaming process was initiated by the reaction of internal constituents in the lead-zinc mine tailings. Different pore structures indicated different foaming mechanisms that probably occurred at different temperatures. The porous ceramics with 60 wt% fly ash addition exhibited excellent properties, including bulk density of 0.93 g/cm³, porosity of 65.6%, and flexural strength of 11.9 MPa.     

Dry pressed ceramic tiles based on fly ash–clay body: Influence of fly ash granulometry and pentasodium triphosphate addition

Fly ash from brown coal (70 wt.%) and stoneware clay (30 wt.%) were used for the dry pressed ceramic tiles (according to EN 14411) raw materials mixture. The effects of fly ash milling and pentasodium triphosphate addition as a deflocculant and fluxing agent on the properties of green body (flexural strength, bulk density) and fired body (EN ISO 10545—water absorption, bulk density, true density, apparent porosity, flexural strength, frost resistance) were studied and explained as a function of the firing temperature (1000–1150 °C). Fly ash milling (corresponding to 5 wt.% residue of fly ash grains on 0.063 mm sieve) increased the sintering abilities of the fly ash–clay body. A similar effect was achieved by 1.3 wt.% pentasodium triphosphate (PST) addition with an increase in green body flexural strength and a decrease in water content of the granulate. Fly ash–clay bodies can be frost resistant with water absorption above 10% due to positive pore size distribution, which were examined using the high-pressure mercury porosimetry method.     

Improving compressive strength of fly ash-based geopolymer composites by basalt fibers addition

In this study, ASTM Class C fly ash used as an alumino-silicate source was activated by metal alkali and cured at low temperature. Basalt fibers which have excellent physical and mechanical properties were added to fly ash-based geopolymers for 10–30% solid content to act as a reinforced material, and its influence on the compressive strength of geopolymer composites has been investigated. XRD study of synthesized geopolymers showed an amorphous phase of geopolymeric gel in the 2θ region of 23°–38° including calcium-silicate-hydrate (C-S-H) phase, some crystalline phases of magnesioferrite, and un-reacted quartz. The microstructure investigation illustrated fly ash particles and basalt fibers were embedded in a dense alumino-silicate matrix, though there was some un-reacted phase occurred. The compressive strength of fly ash-based geopolymer matrix without basalt fibers added samples aged 28 days was 35 MPa which significantly increased 37% when the 10 wt%. basalt fibers were added. However, the addition of basalt fibers from 15 to 30 wt% has not shown a major improvement in compressive strength. In addition, it was found that the compressive strength was strong relevant to the Ca/Si ratio and the C-S-H phase in the geopolymer matrix as high compressive strength was found in the samples with high Ca/Si ratio. It is suggested that basalt fibers are one of the potential candidates as reinforcements for geopolymer composites development.     

Bond strength between blended slag and Class F fly ash geopolymer concrete with steel reinforcement

In this paper, geopolymer concrete bond with both deformed and smooth reinforcing steel bars is investigated using the standard RILEM pull-out test. The geopolymer binder is composed of 85.2% of low calcium fly ash and 14.8% of ground granulated blast furnace slag (GGBFS). The tests were aimed to assess the development of the bond strength from 24 h to 28 days after casting, with different heat curing conditions. The results show that 48 h of heat curing at 80 °C is required in order to obtain similar or better performances to those of the reference 45 MPa OPC concrete. The 28-day bond strength and the overall bond stress–slip behaviour of the geopolymer concrete were similar to those previously reported for OPC-based concretes. Providing intensive heat curing, high early bond strength can be achieved showing that Class F fly ash geopolymer concrete is well suited for precast applications.     

A kinetic study of gaseous potassium capture by coal minerals in a high temperature fixed-bed reactor

The reactions between gaseous potassium chloride and coal minerals were investigated in a lab-scale high temperature fixed-bed reactor using single sorbent pellets. The applied coal minerals included kaolin, mullite, silica, alumina, bituminous coal ash, and lignite coal ash that were formed into long cylindrical pellets. Kaolin and bituminous coal ash that both have significant amounts of Si and Al show superior potassium capture characteristics. Experimental results show that capture of potassium by kaolin is independent of the gas oxygen content. Kaolin releases water and forms metakaolin when heated at temperatures above 450 °C. The amounts of potassium captured by metakaolin pellet decreases with increasing reaction temperature in the range of 900–1300 °C and increases again with further increasing the temperature up to 1500 °C. There is no reaction of pre-made mullite with KCl at temperatures below 1300 °C. However, the weight gain by mullite is only slightly smaller than that by kaolin in the temperature range of 1300–1500 °C. A simple model was developed for the gas–solid reaction between potassium vapor and metakaolin pellet at 900 °C.     

Thin fly ash/ ladle furnace slag geopolymer: Effect of elevated temperature exposure on flexural properties and morphological characteristics

The flexural properties and thermal performance of 10 mm-thin geopolymers made from fly ash and ladle furnace slag were evaluated before and after exposure to elevated temperatures (300 °C, 600 °C, 900 °C, 1100 °C and 1150 °C). Class F fly ash was mixed with liquid sodium silicate (Na₂SiO₃) and 12 M sodium hydroxide (NaOH) solution using aluminosilicate/activator ratio of 1:2.5 and Na₂SiO₃/NaOH ratio of 1:4 to synthesise thin fly ash (FA) geopolymers. 40 wt% of ladle furnace slag was partially replacing fly ash to produce fly ash/slag-based (FAS) geopolymers. Thermal treatment enhanced the flexural strength of thin geopolymers. In comparison to the unexposed specimen, the flexural strength of FA geopolymers at 1150 °C and FAS geopolymers 1100 °C was increased by 161.3% to 16.2 MPa and 208.9% to 24.1 MPa, respectively. A more uniform heating was achieved in thin geopolymers which favoured the phase transformation at high temperatures and contributed to the substantial increase in flexural strength. The joint effect of elevated temperature exposure and the incorporation of ladle furnace slag further improved the flexural strength of thin geopolymers. The calcium-rich slag refined the pore structure and increased the crystallinity of thin geopolymers which aided in high strength development.     

Hydration of Portland cement with high replacement by siliceous fly ash

The effects of two different low calcium fly ashes on the hydration of ordinary Portland cement (OPC) pastes containing 50 wt.% of fly ash were investigated over a hydration time of 550 days. The results were compared with a reference blend of OPC containing 50 wt.% of inert quartz powder allowing the distinction between "filler effect" and pozzolanic reaction.Until 2 days, no evidence of fly ash reaction was measured and its influence on the hydration is mainly related to the “filler effect”. From 7 days on, the effects of the pozzolanic reaction were observed by the consumption of portlandite, the change of the pore solution chemistry, the formation of a presumably water-rich inner hydration product and the change of the C–S–H composition towards higher Al/Si ratio compared to the C–S–H of neat OPC. Additional strength due to the pozzolanic reaction developed after 28 days of hydration.     

Sintered esseneite–wollastonite–plagioclase glass–ceramics from vitrified waste

Dense sintered esseneite–wollastonite–plagioclase glass–ceramics have been successfully prepared from a vitrified mixture of important inorganic waste (Bayer process red mud, fly ash from lignite combustion and residues from the polishing of porcelain stoneware tiles). The enhanced nucleation activity of fine glass powders, favoured by particular oxidation conditions, caused a substantial crystallisation, even in the case of very rapid thermal treatments at 900 °C, which led to remarkable mechanical properties (bending strength and Vickers micro-hardness exceeding 130 MPa and 7 GPa, respectively) and a promising chemical durability.     

Metakaolin and fly ash alkali-activated mortars compared with cementitious mortars at the same strength class

Alkali-activated and cementitious mortars belonging to R1 ≥ 10 MPa, R2 ≥ 15 MPa and R3 ≥ 25 MPa strength classes were tested and compared in terms of workability, dynamic modulus of elasticity, porosimetry, and water vapor permeability. Capillary water absorption, drying shrinkage, resistance to sulfate attack, and corrosion behavior of embedded bare and galvanized reinforcements were also investigated.In alkali-activated mortars, drying shrinkage is higher than that of cementitious mortars but restrained shrinkage is lower due to lower modulus of elasticity. Pore dimensions affect water vapor permeability, more pronounced in alkali-activated mortars, and capillary water absorption, much lower in fly ash ones. The high alkalinity of fly ash and metakaolin mortars delayed the achievement of the passive state in particular for the galvanized reinforcements but after 1 month of curing they reached the same corrosion rates of those embedded in cementitious mortars.     

The effect of grinding process on mechanical properties and alkali–silica reaction resistance of fly ash incorporated cement mortars

The effect of fineness of fly ash on mechanical properties and alkali–silica reaction resistance of cement mortar mixtures incorporating fly ash has been investigated within the scope of this study. Blaine fineness of fly ash has been increased to 907 m²/kg from its original 290 m²/kg value by a ball mill. Test samples were prepared by replacing cement 20, 40 and 60%, with finer and coarser fly ashes and kept under standard and steam curing conditions until testing. Test results showed that grinding process improved the mechanical properties of all samples significantly. The beneficial effect of grinding fly ash, may increase utilization of this by-product in precast and ready-mix concrete industries. Incorporation of fly ash with different fineness values and ratios also decreased the expansions to harmless levels of cement mortars due to alkali–silica reaction.     

Synthesis of glass-ceramics using glass cullet and vitrified industrial by-products

This study concerns the recycling of inorganic waste materials for the production of glass-ceramics and the evaluation of the developed physical properties. Four industrial by-products were selected due to their mass production: (i) two high calcium lignite fly ashes, (ii) slag derived from the production of Fe–Ni and, (iii) steel slag. In order to examine the role of the SiO₂ in the crystallization process, glass cullet and Egyptian sand were added. Thermal treatment, at 1450 °C, enables the production of glasses using mixtures of these materials at appropriate proportions. The crystallization was achieved by heating at 900, 950 and 1000 °C. The produced materials were examined concerning their structure by X-ray diffraction and scanning electron microscopy (SEM-EDS). The results showed that the crystalline phase is greatly depending on the structure of the raw material and the thermal process, influencing accordingly the hardness of the final products.     

Mineralogy and phase transition of oil sands coke ash

Coke obtained from Syncrude and Suncor was investigated to characterize the metals and minerals by ashing it at various temperatures. Samples were collected by high temperature ashing at 100 °C intervals from 400 to 1200 °C. Samples were also obtained from low temperature ashing (LTA) which gives little effect on the mineral assemblage compared to HTA samples. X-ray diffraction patterns of Suncor and Syncrude coke ash were analyzed qualitatively and quantitatively to characterize the mineral phases in the sample and their thermal transition behavior. In Suncor ash, kaolinite, illite, gypsum, anhydrite, microcline, anorthite, hematite, sillimanite and quartz were dominant phases in ash from the LTA temperature up to 700 °C, and mullite, cristobalite, hercynite, albite, anorthite, pseudobrookite and other iron–titanium oxides were dominant mineral phases from 700 to 1200 °C. In Syncrude ash, illite, anhydrite, quartz, anorthite, microcline, sillimanite and hematite were dominant up to 700 °C, and hercynite, anorthite, albite, pseudobrookite and other iron–titanium oxides were dominant up to 1200 °C. The higher quantities of Ca, K and Na, and the lower quantities of V, Fe and Ni in Syncrude ash resulted in higher amorphocity and the different mineral phases.     

Characterization of coal fly ash for possible utilization in glass production

The recycling of three different fly ashes obtained from the coal fired thermal power plants has been studied. Coal fly ashes were vitrified by melting them at 1773 K for 5 h without any additives. After the glass production, glass samples were subjected to a heat treatment process to be able to see whether or not the glasses could be transformed into a microcrystalline structured materials. Produced glass samples were heated to 1423 K and held at this temperature for 2 h to determine the effect of heat treatment process on the properties of glasses. The properties of glass and the heat treated glass samples produced from coal fly ash were investigated by means of differential thermal analysis (DTA), X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. DTA study indicated that there were only inflection points of the endothermic peaks in the DTA curves of the glass samples. XRD analysis showed the amorphous state of the glass samples and also the presence of only the diopside phase in the heat-treated glass samples. SEM investigations revealed that small amount of crystallites occurred in the microstructure of the heat treated glass samples in contrast to the amorphous structure of the glass samples. The mechanical, physical and chemical properties of the heat-treated glass samples are found better than those of the glass samples. Toxicity characteristic leaching procedure (TCLP) results showed that the heavy metals of fly ashes were successfully immobilized into both glass and heat treated glass samples. It can be said that glass and heat treated glass samples obtained by the recycling of coal fly ash can be taken as a non-hazardous material. Overall, results indicated that the vitrification technique is an effective way for the stabilization and recycling of coal fly ash.     

Recycling of lime mud and fly ash for fabrication of anorthite ceramic at low sintering temperature

Lime mud is a kind of waste generated during causticization reaction of an alkali recycling process in paper industry. Lime mud and fly ash were reused as raw materials to fabricate anorthite ceramics through solid state reactions. Both sintering temperature and lime mud content influenced the crystalline phases in the prepared ceramics. Anorthite was the major phase in all samples (samples L36, L40, L50 and L60) and it was prominent in sample L36 (containing 36 wt% lime mud). The results also showed that anorthite ceramic can be synthesized at low sintering temperature (1100 °C). Gehlenite and wollastonite were formed in the samples possessing higher calcium (above 40 wt% lime mud) or at lower sintering temperatures. Bulk density, water absorption and compressive strength were measured. These ceramics were of light weight and had high water absorption. Recycling of lime mud and fly ash as raw materials of anorthite ceramic is a feasible approach to solve the solid wastes.     

Synthesis of volcanic ash-based geopolymer mortars by fusion method: Effects of adding metakaolin to fused volcanic ash

The present study aimed at improving the properties of geopolymer mortars obtained from volcanic ash as a source material. An alkali fusion process was used to promote the dissolution of Si and Al species from the volcanic ash and thus to enhance the reactivity of volcanic ash. Various amount of metakaolin (30%, 40%, 50% and 60% MK by weight) was used to consume the excess alkali needed for the fusion. The amount of amorphous phase was determined both in the volcanic ash and the fused volcanic ash and X-ray diffraction analysis was used to evaluate effect of the alkaline fusion method. Geopolymers were prepared by alkali activation of mixtures of powders of fused volcanic ash, various amount of metakaolin and river sand using a sodium silicate solution as activator. The geopolymer mortars were characterized by determination of setting time, linear shrinkage, scanning electron microscopy and compressive strength. The results of this study indicate that geopolymer mortars synthesized by the fusion method exhibit low setting time (7–15 min), low shrinkage (0–0.42%) and high compressive strength (41.5–68.8 MPa). This study showed that, by enhancing the reactivity of volcanic ash by alkali fusion and balancing the Na/Al ratio through the addition of metakaolin, all volcanic ashes can be recycled as an alternative source material for the production of geopolymers.     

Sinterability,microstructure and compressive strength of porous glass-ceramics from metallurgical silicon slag and waste glass

Porous glass-ceramics have been prepared by the direct sintering of powder mixtures of metallurgical silicon slag and waste glass. The thermal behavior of silicon slag was examined by differential thermal analysis and thermogravimetry to clarify the foaming mechanism of porous glass-ceramics. The mass loss of silicon slag below 700 °C was attributed to the oxidation of amorphous carbon from residual metallurgical coke in the silicon slag, and the mass gain above 800 °C to the passive oxidation of silicon carbide. The porosity of sintered glass-ceramics was characterized in terms of the apparent density and pore size. By simply adjusting the content of waste glass and sintering parameters (i.e. temperature, time and heating rate), the apparent density changed from 0.4 g/cm³ to 0.5 g/cm³, and the pore size from 0.7 mm to 1.4 mm. In addition to the existing crystalline phases in the silicon slag, the gehlenite phase appeared in the sintered glass-ceramics. The compressive strength of porous glass-ceramics firstly increased and then decreased with the sintering temperature, reaching a maximal value of 1.8 MPa at 750 °C. The mechanical strength was primarily influenced by the crystallinity of glass-ceramics and the interfaces between the crystalline phases and the glassy matrix. These sintered porous glass-ceramics exhibit superior properties such as light-weight, heat-insulation and sound-absorption, and could found their potential applications in the construction decoration.     

Synthesis of a nano-crystalline solid acid catalyst from fly ash and its catalytic performance

The synthesis of nano-crystalline activated fly ash catalyst (AFAC) with crystallite size of 12 nm was carried out by chemical and thermal treatment of fly ash, a waste material generated from coal-burning power plants. Fly ash was chemically activated using sulfuric acid followed by thermal activation at 600 °C. The variation of surface and Physico-chemical properties of the fly ash by activation methods resulted in improved acidity and therefore, catalytic activity for acid catalyzed reactions. The AFAC was characterized by X-ray diffraction, FT-IR spectroscopy, N₂-adsorption–desorption isotherm, scanning electron microscopy, flame atomic absorption spectrophotometry and sulfur content by CHNS/O elemental analysis. It showed amorphous nature due to high silica content (81%) and possessed high BET surface area (120 m²/g). The catalyst was found to be highly active solid acid catalyst for liquid phase esterification of salicylic acid with acetic anhydride and methanol giving acetylsalicylic acid and methyl salicylate respectively. A maximum yield of 97% with high purity of acetylsalicylic acid (aspirin) and a very high conversion 87% of salicylic acid to methyl salicylate (oil of wintergreen) was obtained with AFAC. The surface acidity and therefore, catalytic activity in AFAC was originated by increased silica content, hydroxyl content and higher surface area as compared to fly ash. The study shows that coal generated fly ash can be converted into potential solid acid catalyst for acid catalyzed reactions. Furthermore, this catalyst may replace conventional environmentally hazardous homogeneous liquid acids making an ecofriendly; solvent free, atom efficient, solid acid based catalytic process. The application of fly ash to synthesize a solid acid catalyst finds a noble way to utilize this abundant waste material.     

Preparation and characterization of the one-piece wall ceramic board by using solid wastes

For the purpose of building energy-saving, a novel one-piece wall ceramic board was prepared by using fly ash and ceramic waste as the main raw materials for its matrix part and foam part, respectively. The effects of raw material composition, sintering temperature on the macro and micro properties were systematically investigated. The optimum parameter for the matrix part was obtained at 1220 °C with 70 wt% fly ash and 4 wt% quartz, while that for the foam part was 1220 °C with 97 wt% ceramic waste and 3 wt% silicon carbide. For the matrix sample, the highest rupture modulus reaches 53.97 MPa, and the corresponding water absorption capacity and thermal conductivity are 1.08% and 0.54396 W/(m K), respectively. For the foam part, the best bulk density and thermal conductivity are 443 kg/m³ and 0.10528 W/(m K), respectively. Subsequently, the optimal matrix and foam samples were introduced into the co-fired process (1220 °C), and the results show that the new method for the preparation of one-piece wall ceramic board was fully acceptable. Furthermore, the simulated results indicate that the proposed one-piece wall ceramic board can efficiently reduce the thermal bridges and exerts excellent energy conservation effect.