Monoclinic (Celsian) and hexagonal (Hexacelsian) Ba 1 _ JC Sr JC Al 2 Si 2 0 8 solid solutions, where x = 0,0.25,0.375,0.5,0.75 or 1, were synthesized by using Coal Fly Ash (CFA) as main raw material, employing a simple one-step solid-state reaction process involving thermal treatment for 5 h at 850-1300 °C. Fully monoclinic Celsian was obtained at 1200 °C/5 h, for SrO contents of 0.25 < x < 0.75. However, an optimum SrO level of 0.25 < x < 0.375 was recommended for the stabilization of Celsian. These synthesis conditions represent a significant improvement over the higher temperatures, longer times and/or multi-step processes needed to obtain fully monoclinic Celsian, when other raw materials are used for this purpose, according to previous literature. These results were attributed to the role of the chemical and phase constitution of CFA as well as to a likely mineralizing effect of CaO and Ti0 2 present in it, which enhanced the Hexacelsian to Celsian conversion.
Celsian with a chemical composition of Ba0.75Sr0.25Al2Si2O8, is synthesized by using coal fly ash (byproduct of a Mexican coal-burning power plant, composed mainly by SiO2 and Al2O3) as main raw material. The thermal behavior of the synthesized material is evaluated by differential (DTA) and gravimetric (TGA) thermal analyses as well as by heating microscopy; its coefficient of linear thermal expansion (CTE) is also determined. Heating microscopy shows that cylinders of compacted powdered Celsian start sintering at ∼1140 ºC, which is associated with a considerable contraction occurring up to 1500 ºC. The mean CTE value of the material in the temperature range of 30-1100ºC is slightly affected by the synthesis conditions employed. Synthesis at 1400 or 1300 ºC during 10 h, with a pre-calcination step at 900 ºC/5h in both cases, produce mean CTE values of 5.15 x 10-6 and 5.43 x 10-6 ºC-1, respectively. On the other hand, Celsian synthesized at 1400 ºC/10 h, without the pre-calcination step, has a mean CTE value of 5.25 x 10-6 ºC-1. Lastly, the DTA/TGA analysis of the synthesized material shows that a slight weight gain takes place from room temperature to 1100ºC, which is followed by a slight weight loss up to 1300ºC. This is attributed to oxidation and evaporation of some of the impurities present in the material.
Two alternative chemical methods are studied for the extraction of Al2O3 from Mexican Fly Ash (FA). Reaction of FA with H2SO4 at high temperature allows extracting ∼37% of the total Al2O3 contained in the FA as Al2(SO4)3, regardless of H2SO4 concentration, treatment time and temperature employed. This is partly due to the high chemical resistance of mullite (Al6Si2O13) contained in the FA. In contrast, reaction of FA with a CaCO3-Na2CO3 mixture at 1300°C/1h, followed by lixiviation with a Na2CO3 aqueous solution and precipitation of bohemite [AlO(OH)] by addition of either H2O2 or NH4HCO3, allows extracting ∼80% of the total Al2O3 contained in the FA as θ-alumina, after calcination of bohemite at 1200°C/1h.
Four Celsian (Ba0.75Sr0.25Al2Si2O8)/Mullite (Al6Si2O13) composites, with potential structural applications at high temperatures, are synthesized from coal fly ash (byproduct of a Mexican coal-burning power plant, constituted mainly by SiO2 and Al2O3). Nominal Celsian/Mullite weight ratios studied are 80/20, 60/40, 40/60 and 20/80. Mullite is synthesized separately at 1600ºC/2h and then mixed with a Celsian precursor mixture previously calcined at 900°C/5h. During this process the Celsian phase is formed by a solid state reaction at 1100-1400ºC/5h. Prior to this, the reacting mixture is milled in a planetary mill during 1 or 2h and then compacted by uniaxial and cold isostatic pressing. The microstructure and phase composition of the synthesized composites are characterized by X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM/EDS). Their dynamic Young’s modulus is measured by an ultrasonic technique, and their mechanical strength is evaluated from flexural tests carried out at room temperature. The expected phases are obtained in all cases, although with some differences with respect to their expected relative proportions, according to the studied nominal compositions. In general, the longest milling time employed produced samples with the largest degree of crystallinity and density, as well as with the best microstructural characteristics and mechanical properties.
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