Analysis of silica fume produced by zircon desilication

Novel chemical methods have been developed to allow for the determination of the components of silica fume produced by zircon desilication. Hitherto, no methods have been described for the analysis of this material. The amorphous silica is first removed by treatment with sodium hydroxide. The residue from the hydroxide treatment may then be subjected to a suite of reagents to determine the zircon, the total zirconia, the monoclinic zirconia and the tetragonal zirconia content of the fume. The zircon content of the fume is determined by treatment of the hydroxide residue with concentrated hydrofluoric acid (HF). The total zirconia content of the fume is determined by digestion of the hydroxide residue with fuming sulphuric acid (oleum), while the relative amounts of monoclinic and tetragonal zirconia may be found by treatment of the hydroxide residue with 10%w/v HF, which attacks the less stable tetragonal phase. Both X-ray diffraction and particle size analysis were used to validate the steps in the analytical procedure. An explanation of the presence of tetragonal zirconia in the fume is proposed. A greater understanding of the composition of the fume led to the installation of a separator in the company's production line to remove the zircon. Australian Fused Materials (AFM) now produces a vastly superior grade of fume marketed under the code SF-98.     

Gravimetric determination of free carbon and silicon carbide in silica fume

Silica fume is formed as a by-product in the manufacture of silicon from quartzite. This paper describes an analytical method for the determination of free carbon and silicon carbide in silica fume. The silicon carbide was determined after removal of free carbon, amorphous silica, crystalline silica, graphite and silicon from the fume. The free carbon content was found to vary from 2 to 8% while the silicon carbide content ranged from 1 to 5%. X-ray diffraction, thermal analysis, scanning electron microscopy and Fourier Transform infrared spectroscopy were used to validate the steps used in the analytical procedure. The purpose of determining the free carbon and silicon carbide content of the fume is to help understand the efficiency of the reduction process and mechanism of the reaction.     

Calorimetric comparison of portland cements containing silica fume and metakaolin

This new study must be regarded to be a direct outcome of two previous studies published by these same authors, which were conducted to respond to interesting questions brought out about the effect of silica fume, SF and metakaolins, M and MQ, on the heat of hydration of portland cements, PC, with very different C₃A and C₃S contents. The answer to these so interesting questions has been the primary objective of the present research. For this purpose, the same PC, PC1 (14% C₃A) and PC2 (≈0% C₃A), metakaolins, silica fume and blended cements were once again used more 60/40 for sulphate attack, and the same analytical techniques (CC, pozzolanicity and XRD analysis) and parameters determined as well. In this new research, the sulphate attack was determined by two accelerated methods: Le Chatelier-Ansttet and ASTM C 452-68. The experimental results of sulphate attack mainly, have demonstrated definitively that the high, rapid and early pozzolanic activity exhibited by SF also is, as in the case of the two metakaolins, more specific than generic, for it indirectly stimulated greater C₃A than C₃S hydration, but only in the first 16 h monitored in this study. Thereafter it is the contrary, i.e., anti- or contra-specific for the same purpose. And the longer the hydration time, the more anti- or contra-specific it became, since, when exposed to sulphate attack, SF blended cements resisted or even prevented the aggressive attack against PC1 which, with a higher C₃A content than PC2, was the more vulnerable of the two. By contrast, metakaolin MQ not only failed to hinder or prevent the attack, but heightened its effects, rendering it more intense, aggressive and rapid, leading to what could be called a rapid gypsum attack.     

Calorimetry of portland cement with silica fume and gypsum additions

The use of active mineral additions is an important alternative in concrete design. Such use is not always appropriate, however, because the heat released during hydration reactions may on occasion affect the quality of the resulting concrete and, ultimately, structural durability. The effect of adding up to 20% silica fume on two ordinary Portland cements with very different mineralogical compositions is analyzed in the present paper. Excess gypsum was added in amounts such that its percentage by mass of SO₃ came to 7.0%. The chief techniques used in this study were heat conduction calorimetry and the Frattini test, supplemented with the determination of setting times and X-ray diffraction. The results obtained showed that replacing up to 20% of Portland cement with silica fume affected the rheology of the cement paste, measured in terms of water demand for normal consistency and setting times; the magnitude and direction of these effects depended on the mineralogical composition of the clinker. Hydration reactions were also observed be stimulated by silica fume, both directly and indirectly – the latter as a result of the early and very substantial pozzolanic activity of the addition and the former because of its morphology (tiny spheres) and large BET specific surface. This translated into such a significant rise in the amounts of total heat of hydration released per gram of Portland cement at early ages, that silica fume may be regarded in some cases to cause a synergistic calorific effect with the concomitant risk of hairline cracking. The addition of excess gypsum, in turn, while prompting and attenuation of the calorimetric pattern of the resulting pastes in all cases, caused the Portland cement to generate greater heat of hydration per gram, particularly in the case of Portland cement with a high C₃A content.     

Sintering of silica fume in furnace atmospheres with controlled water vapour partial pressure

Sintering process of compacted silica fume samples with respect to various water vapour partial pressures (p _total=101 kPa) within the furnace atmosphere has been characterized by means of dilatometry and bulk density measurements. Dilatometric study shows the strong dependence of sintering process on the water vapour partial pressure. Water vapour intensifies the process and affects relative densities of the final product, as well.The work was supported by Grant No. 930 of the Ministry of Education and Science of the Slovak Republic.     

纳米硅粉/MC尼龙6复合材料的制备与性能

将纳米硅粉分散于熔融的己内酰胺中,以NaOH为催化剂,2,4-甲苯二异氰酸酯为助催化剂,原位制备了纳米硅粉/MC尼龙6复合材料.用红外光谱、X射线衍射、场发射扫描电镜、热重分析仪和差示扫描量热仪对复合材料的界面结构和性能进行了研究.结果表明,纳米硅粉在尼龙6基体中具有较好的分散性,而且其与基体有比较强的界面作用,纳米硅粉促进了尼龙6的结晶,但是其对尼龙6的晶型结构没有产生明显的影响.     

Microstructure development in mixes of calcium aluminate cement with silica fume or fly ash

The most widely identified degradation process suffered by calcium aluminate cement (CAC) is the so-called conversion of hexagonal calcium aluminate hydrate to cubic form. This conversion is usually followed by an increase in porosity determined by the different densities of these hydrates and the subsequent loss of strength. Mixes of calcium aluminate cement (CAC) and silica fume (SF) or fly ash (FA) represent an interesting alternative for the stabilization of CAC hydrates, which might be attributed to a microstructure based mainly on aluminosilicates. This paper deals with the microstructure of cement pastes fabricated with mixtures CAC-SF and CAC-FA and its evolution over time. Thermal analysis (DTA/TG), X-ray diffraction (XRD) and mid-infrared spectroscopy (FTIR) have been used to assess the microstructure of these formulations.     

Artificial pozzolanic cement pastes containing burnt clay with and without silica fume

Pozzolanic cement blends were prepared by the partial substitution of ordinary Portland cement (OPC) with different percentages of burnt clay (BC), Libyan clay fired at 700 °C, of 10, 20, and 30%. The pastes were made using an initial water/solid ratio of 0.30 by mass of each cement blend and hydrated for 1, 3, 7, 28, and 90 days. The pozzolanic OPC–BC blend containing 30% BC was also admixed with 2.5 and 5% silica fume (SF) to improve the physicomechanical characteristics. The hardened pozzolanic cement pastes were subjected to compressive strength and hydration kinetics tests. The results of compressive strength indicated slightly higher values for the paste made of OPC–BC blend containing 10% BC The results of DSC and XRD studies indicated the formation and later the stabilization of calcium silicates hydrates (CSH) and calcium aluminosilicate hydrates (C₃ASH₄ and C₂ASH₈) as the main hydration products in addition to free calcium hydroxide (CH). Scanning electron microscopic (SEM) examination revealed that the pozzolanic cement pastes made of OPC–BC mixes possesses a denser structure than that of the neat OPC paste. Furthermore, the addition of SF resulted in a further densification of the microstructure of the hardened OPC–BC–SF pastes; this was reflected on the observed improvement in the compressive strength values at all ages of hydration.     

Synergistic effect of nano-silica and silica fume on hydration properties of cement-based materials

Journal of Thermal Analysis and Calorimetry - Synergistic effect of nano-silica and silica fume on hydration properties was studied in cement-based materials. In the present study, various tests...     

Determination of amorphous silica and total silica in plant materials

Amorphous silica in plant material was dissolved with potassium carbonate solution, after nitric acid/hydrogen peroxide digestion. Total silica in plant material and some minerals was obtained after ashing and fusing in nickel crucibles with potassium hydroxide containing potassium tetraborate/nitrate. The relative standard deviation for determinations of silicon by these methods in plant material was <2% for plant material containing 2–2100 μmol Si g^?1 (dry weight).     

Direct-on-filter analysis of crystalline silica using photoacoustic Fourier transform-infrared spectroscopy

Photoacoustic Fourier transform-infrared spectroscopy (PA-FT-IR) has been used to perform direct-on-filter (DOF) analysis of crystalline silica using laboratory-generated filter samples. With these samples, the silica particles were embedded in the stable three-dimensional matrix of the filter. In this preliminary study, it was demonstrated that the photoacoustic (PA) signals generated from direct-on-filter measurements were significantly higher than the corresponding signals for equivalent amounts of silica particles placed directly in the photoacoustic detector cup. Studies with Min-U-Sil-5 loaded onto 9 mm filter stubs indicated a limit of detection of less than 10 μg. Additionally, Teflon filters were demonstrated to be more suitable for these measurements than other types. The photoacoustic FT-IR approach seems to be feasible for further development to use with full-sized personal sampling filters.     

High-density storage of H2 in microporous crystalline silica at ambient conditions

Molecular hydrogen was encapsulated in the cages of clathrasil decadodecasil 3R (DD3R) during the hydrothermal synthesis of this microporous silicate. The crystalline structure of DD3R facilitates high-density hydrogen storage at ambient conditions. Prompt gamma activation analysis (PGAA) revealed that on average about one molecule of H2 is trapped in each (5(12)) cage of DD3R. The presence of molecular hydrogen inside the DD3R framework was confirmed by solid-state 1H NMR spectroscopy. Temperature-programmed decomposition (TPD) in combination with mass spectrometry showed that the encapsulated hydrogen is released upon decomposition of the clathrasil structure. This release can be promoted by the presence of water.     

Determination of the molecular symmetry in crystalline germane

The symmetry of the germane molecule in the various crystalline phases of solid germane has been investigated using the IR spectrum of the isotopically dilute GeH₃D molecule. The observed spectra indicate that the cubic crystal symmetry of the higher-temperature phases is lost in phase III and possible site symmetries are proposed. Band broadening is found in phase I and is interpreted as arising from rapid molecular reorientation.     

Shear-induced alignment and nanowire silica synthesis in a rigid crystalline surfactant mesophase

Highly aligned stringlike silica nanostructures are obtained through templated synthesis in the columnar hexagonal structure of a rigid crystalline surfactant mesophase. A two-step procedure is used to first shear-align the surfactant mesophase and then conduct synthesis under quiescent conditions in the mesophase. The mesophase retains its alignment for extended periods, allowing materials synthesis to be decoupled from the application of shear. The observations have significant implications in the control of ceramic microstructure morphology and transitions from nonaligned to aligned nanowire type structures.     

Close-packed colloidal crystalline arrays composed of silica spheres coated with titania

Titania coated monodisperse silica spheres have been synthesized and fabricated as a close-packed colloidal crystalline array. We have demonstrated that the coated colloidal sphere can be used to control the peak position of the optical stop band through variation of the coating thickness. The titania coated silica spheres were prepared by the layer-by-layer assembly coating process, which reciprocally laminates the cationic polyelectrolyte and the anionic titania nanosheets on a monodisperse silica spheres, and were sintered to change the titania nanosheets to anatase. The Bragg diffraction peak of the colloidal crystalline array shifted to the long wavelength region with an increase of thickness of the titania layer. Angle-resolved reflection spectra measurements clarified that the red shift was caused by increasing of the refractive index with increase of the thickness of the layer. The current work suggests new possibilities for the creation of advanced colloidal crystalline arrays with tunable optical properties from tailored colloidal spheres.     

Influence of silica fume on radioactive fluoride concentrate liquid waste solidified by magnesium potassium phosphate cement

Journal of Radioanalytical and Nuclear Chemistry - This paper investigated the influence of silica fume on radioactive fluoride concentrate liquid waste cementation with magnesium potassium...     

Comparison of long-range activation transfer in gamma-radiolysis of single crystalline quartz with amorphous silica

Gamma-radiolysis of single crystalline quartz and amorphous fused silica of high purity was studied at 77 K by ESR spectroscopy. The aluminium-hole centers ([Al_e+]°) in the γ-irradiated quartz, appear at doses as low as 250 rad. Their yields increase with increasing dose and reach plateau values at approx. 10⁴ rad. The yields of the radiation damages, such as the oxygen-associated hole centers, E' centers and H atoms, in γ-irradiated silica, however, increase with increasing dose up to 5 x 10⁶ rad without reaching plateau values. The [Al_e+]° centers in quartz are also produced by illumination with 185 nm light. The G-values of radiation damages in quartz and silica were measured. The efficient production of the [Al_e+]° centers in the γ-irradiated quartz was interpreted in terms of long-range migration of mobile entities, such as a hole and an exciton. The migration range was estimated from the G-values and concentration of impurities. It has turned out that the mobile entities in quartz migrate through 10⁴-10⁵SiO₂ units, whereas those in silica migrate only through 5-50 SiO₂ units.     

Determination of silica in glasses,ceramics and refractories

A rapid method for the determination of silica in glasses, glass ceramics and refractories is described. The utilization of direct coulometric titration of the excess of 8-quinolinol employed to precipitate the silico-12-molybdate complex, enables duplicate determinations in the presence of diverse ions to be completed in about 3h. Studies of the optimum, conditions indicated that the acidity and choice of acid were critical. For greatest versatility a sulfuric acid medium was better than hydrochloric or perchloric acids. The addition of glycerol allowed analysis of titanium-containing refractories. The accuracy of the method for a wide variety of materials is similar to that of the conventional acid-dehydration method.