The recycling of MSWI bottom ash in silicate based ceramic

The possibility of recycling the Municipal Solid Wastes Incinerated (MSWI) bottom ash by its incorporation in ceramic tiles was investigated. The MSWI bottom ash was introduced both in untreated (previous deironization) and vitrified condition. The sintering of the different products was investigated by determining water absorption and linear shrinkage. To evaluate possible variations due to the presence of different amount of bottom ash, mineralogical and microstructural examinations by quantitative X-ray diffraction and scanning electron microscopy, were performed. While the untreated bottom ash, till an amount of 5 wt%, did not seem to affect the above characteristics of selected materials, the vitrified bottom ash, 5–10 wt%, as strong fluxing agent, promoted the sintering of porcelain stoneware. Leaching results allow to assert that the fired samples are not dangerous.     

Dry sliding wear of zirconia-toughened alumina with different metal oxide additives

Tribological behaviour of zirconia-toughened alumina (ZTA) with different metal oxide additives was studied. Solid oxide lubricants (MO_x; M = Cu, Ti, Mg, Zn, Mn) were added in small quantities (∼8–11 wt%) to provide a self-lubrication action and thereby to decrease the coefficient of dry friction. Dry mixed ceramic composites powders were compacted and pressureless sintered at different temperatures. Densification studies show that near full densities (>97%) were obtained for ZTA ceramic containing both TiO₂–CuO and TiO₂–MnO₂ at 1450 °C. Phase and qualitative compositional analysis was done using X-ray diffraction (XRD) and energy-dispersive spectroscopy (EDS). Tribological behaviour of the various ZTA composites was tested by dry sliding the different specimens against SiC abrasive grit paper at a load of 50 N. The lowest specific wear rate of 9.2 × 10⁻⁵ mm³/N m and coefficient of friction of 0.35 were observed for the ZTA ceramic composite with TiO₂–MnO₂. The basic wear mechanisms were abrasion and grain pullout as corroborated from scanning electron microscopy (SEM) images.     

Pore structure of carbons coated on ceramic particles

Pore structure of carbon coated on ceramic particles by carbonization of precursor in a powder mixture at 900 °C was studied by focusing on the effects of substrate ceramics (MgO, TiO₂ and various phases of Al₂O₃) and of carbon precursor (poly(vinyl alcohol) (PVA), poly(ethylene terephthalate) (PET) and hydroxyl propyl cellulose (HPC)). By dissolving substrate MgO particles, carbon coated was found to have a high BET surface area, more than 1000 m²/g, which was almost the same as the value estimated from apparent surface area measured on carbon-coated MgO particles under the assumption of zero surface area of the substrate. The carbon separated was found to be rich in micropores from the analyses by DFT method and α_s plot. The dependence of the BET surface area on the amount of carbon coated on TiO₂ with a high surface area was the same for three carbon precursors, although the carbon yields from the precursors were slightly different. Porous Al₂O₃ substrates, γ-Al₂O₃as-received and that formed from Al(OH)₃ during carbonization, gave a high BET surface area, but dense Al₂O₃, α-Al₂O₃, gave a low surface area.     

Dielectric characteristics of donor-acceptor modified BaTiO3 ceramics

Sm/Mn codoped BaTiO₃ ceramics were investigated for their microstructure and dielectric characteristics. The powders were prepared by the conventional solid state procedure. The concentration of Sm₂O₃ as a donor dopant has been kept from 0.1 up to 5.0 at%. The content of MnO₂ as acceptor was kept constant at 0.05 at% Mn in all samples. The specimens were sintered at 1290 °C, 1320 °C and 1350 °C in an air atmosphere for two hours.A mainly uniform and homogeneous microstructure with average grain size ranging from 0.3 µm to 2.0 µm was observed in low doped samples. In highly doped samples, apart from the fine grained matrix, the appearance of local area with secondary abnormal grains was observed.The dielectric properties were investigated as a function of frequency and temperature. The low doped samples exhibit the high value of dielectric permittivity at room temperature and the greatest change at the Curie temperature. The highest value of dielectric constant (ε_r=6800) was measured for 0.1Sm/BaTiO₃ samples sintered at 1350 °C. A nearly flat permittivity-temperature response and lower values of ε_r were obtained in specimens with 2.0 and 5.0 at% additive content. The dielectric constant increases with the increase of sintering temperature. The dissipation factor ranged from 0.01 to 0.22 and decreases with the increase of sintering temperature. The Curie constant (C), Curie-Weiss temperature (T₀) and critical exponent of nonlinearity (γ ) were calculated using a Curie-Weiss and modified Curie-Weiss law. The highest value of Curie constant (C=9.06·10⁵ K) was measured in 0.1 at% doped samples. The Curie constant decreased with increasing dopant content. The γ values, ranging from 1.001 to 1.58, point out the sharp phase transition in low doped samples, and the diffuse phase transition in heavily doped BaTiO₃ samples.     

Phase analysis and wear behavior of in-situ spark plasma sintered Ti3SiC2

In-situ synthesis of dense near-single phase Ti₃SiC₂ ceramics from 3Ti/SiC/C/0.15Al starting powder using spark plasma sintering (SPS) at 1250 °C is reported. Systematic analysis of the phase development over a range of sintering temperatures (1050–1450 °C) suggested that solid state reactions between intermediate TiC and Ti₅Si₃ phases lead to the formations of Ti₃SiC₂. The effect of starting powder composition on phase development after SPS at 1150 °C was also investigated using three distinct compositions (3Ti/SiC/C, 2Ti/SiC/TiC, and Ti/Si/2TiC). The results indicate that the starting powder compositions, with higher amounts of intermediate phase such as TiC, favor the formation of Ti₃SiC₂ at relatively lower sintering temperature. Detailed analysis of wear behavior indicated that samples with higher percentage of TiC, present either as an intermediate phase or a product of Ti₃SiC₂ decomposition, exhibited higher microhardness and better wear resistance compared to near single phase Ti₃SiC₂.     

Pore structure of activated carbons prepared by carbon dioxide and steam activation at different temperatures from extracted rockrose

The influence of the activation temperature on the pore structure of granular activated carbons prepared from rockrose (Cistus ladaniferus L.), extracted previously into petroleum ether, is comparatively studied. The preparation was carried out by pyrolysis of a char in nitrogen and its subsequent activation by carbon dioxide and steam (flow of water controlled to generate the same mol number per minute of water as well as carbon dioxide/nitrogen) at 700-950°C to 40% burn-off. The techniques applied to study the pore structure were: pycnometry (mercury, helium), adsorption (carbon dioxide, 298 K; nitrogen, 77 K), mercury porosimetry and scanning electron microscopy. The preparation by steam activation, especially at 700°C, yields activated carbons showing a total pore volume larger than those prepared by carbon dioxide activation. The pore structures present the greatest differences when the activations are carried out between 700 and 850°C and closer at higher temperatures. At high temperatures, the decrease of differences in pore development caused by carbon dioxide or steam is attributed to an external burn-off. The micropore structure of each activated carbon is mainly formed by wide micropores. At the lowest activation temperatures, especially at 700°C, steam develops the mesoporosity much more than carbon dioxide. At 950°C, a similar reduction of pore volume in the macropore range occurs.     

Acidic and basic binders for magnesite based aggregate in plaster of tundish

Binders are generally inorganic, organic or organomineral and have an important influence on the performance and corrosion resistance of slag line and deskulling. Since silicate and phosphate binders have some side effects, in this work sulphate binders such as sulphamic acid, H₂NSO₃H; aluminum sulphate, Al₂(SO₄)₃; ammonium sulphate, (NH₄)₂SO₄; magnesium sulphate, MgSO₄; calcium sulphate, CaSO₄; sodium sulphate, Na₂SO₄; and potassium sulphate, K₂SO₄, are investigated. Cold crushing strength at different heat treatments of room temperature, 110 °C, 1100 °C, 1400 °C is measured. Apparent porosity of samples without pulp and bulk density together with pH of the binder solution is evaluated and XRD and SEM studies are performed. Among these sulphate binders MgSO₄ was found to be the best. It is acidic in nature and develops strong bonds to the basic aggregate, MgO, at low temperatures. At high temperatures it dissociates from MgO(s) and SO₃(g) and the remained portion of MgO is the same as host oxide, with no corrosion and easy deskulling. Basic binders such as calcium sulphate, sodium sulphate and potassium sulphate could not strongly bond the MgO aggregates.     

Densification rate and phase structure changes during sintering of zinc titanate ceramics

Densification rate and phase structure changes during sintering of nanosized ZnTiO₃ were studied. Sintering was performed in a dilatometer in two regimes: the first to 900 °C (heating rates 5, 10 and 15 °C/min) and the second to 1200 °C (heating rates 3, 5 and 10 °C/min). XRD analysis of samples sintered at both temperatures combined with Rietveld structure refinement enabled determination of all phases present and their structure parameters. Samples sintered to 900 °C contained ZnTiO₃ and Zn₂TiO₄ with traces of r-TiO₂ (rutile) and Zn₂Ti₃O₈, while samples sintered to1200 °C contained only r-TiO₂ and Zn₂TiO₄. A master sintering curve was defined for sintering to 900 °C enabling determination of the sintering process activation energy as 313 kJ/mol.     

Pore structure alteration of porous carbon by catalytic coke deposition

The feasibility of preparing Carbon Molecular Sieve (CMS) by tailoring pore structure of activated carbon under catalytic cracking of benzene has been examined. In this method, benzene vapour was cracked over metal-impregnated activated carbon particles at 523–773 K. Among the metal catalysts tested, only cobalt exhibited significant cracking activity toward benzene. In this range of temperature coke was originated on the metal surface only, therefore an excessive coke deposition as indicated in non-catalytic process was not observed. The amount of coke and the site of deposition in the pore network were determined to some extent by the metal loading as well as the rate of benzene cracking. Raman spectra indicated that the coke produced was less amorphous than those produced in non-catalytic processes. Only a small loss in micropore volume and surface area was observed after the coke deposition process. The CMS produced was tested for its adsorption characteristics of carbon dioxide and methane. The improvement in the CO₂/CH₄ kinetic selectivity was observed.     

Cellular glass obtained from non-powder preforms by foaming with steam

Cellular glass, or foamed glass, has been obtained as a result of the heating (to 700–800 °C) of heavy and strong preforms formed due to the binding properties of the silicate additives. Durability of the preforms reached 6 MPa at the density of 1.8 g/cm³. The main expanding agent in the composition is steam, which can also be a carbon oxidizer and increase the amount of the evolved gases and decrease the density of the foamed glass obtained. As a result of changing the initial composition structure, the density of the obtained foamed glass varied from 0.14 to 0.6 g/cm³, its breaking strength - from 0.6 to 5.0 MPa. and heat conductivity – from 0.045 to 0.15 W/(m·К), respectively. The speed of expansion of the preforms had an extreme character with the induction period typical for topochemical reactions. The obtained cellular materials possessed a distinct crystalline structure. The experiments showed the possibility of obtaining cellular materials with acceptable properties from different types of glass for the solution of environmental tasks. Various technological methods of obtaining cellular material blocks from preforms of various forms were tested to use them for thermal insulation and facing materials.     

Effects of heat treatment on the physical properties of lightweight aggregate from water reservoir sediment

Lightweight aggregates (LWAs) were produced from water reservoir sediment with added calcium oxide by employing four heat treatments, respectively, at temperatures in the range of 1170-1230 °C. The results show that LWAs produced at temperatures above 1200 °C meet European Union regulation EN-13055-1, which states that the unit weight of LWAs should be lower than 2000 kg/m³. The bulk density was easily lowered by extending the soaking time and increasing the heating rate. The ratio of strength to unit weight of the LWA produced at 1230 °C with a short soaking time and a fast heating rate was near that of a commercial product. The level of water adsorption was below 4%, which increased initially and then decreased due to pore connections and pore sealing. The formation of a glassy phase made the LWAs treated at higher temperature rough and sealed small pores (<0.1 mm) connected to the walls of large pores (>0.2 mm). The mineral phases of the LWAs were quartz, anorthite, and hematite.     

Effects of sintering temperature on microstructure, nitrogen deficiency and densification of spark plasma sintered Mn3Cu0.5Ge0.5N

Single-phase Mn₃Cu_0.5Ge_0.5N bulks were prepared by spark plasma sintering (SPS) in nitrogen atmosphere at different sintering temperatures, and the effects of sintering temperature on microstructure, nitrogen deficiency and densification were studied. It was found that the densification is accompanied by the thermal decomposition of Mn₃Cu_0.5Ge_0.5N. Nitrogen deficiency and porosity due to the thermal decomposition of the compound do not increase with increase of the sintering temperature; the nitrogen deficiency from decomposition is compensated by the diffusion of nitrogen atoms from the N₂ atmosphere. When the two processes reach the balance, minimum nitrogen deficiency of Mn₃Cu_0.5Ge_0.5N is achieved together with the highest densification.     

Effect of boric acid on the porosity of clay and diatomite monoliths

Porous silica ceramics were obtained at low forming pressure (40–80 MPa) and low sintering temperature (850–1300 °C) for 4 h in air. Boric acid was used as a low-cost additive, in the amount of 2 wt%. Relatively high porosities of nearly 40% and 65% are obtained for the samples of clay and diatomite pressed at 40 MPa, and sintered at 1000 °C, respectively. The samples sintered at 1150 °C and 1300 °C have the average pore size diameters in the range of macroporous for clay 0.2–10 μm and for diatomite 0.2–5 μm. X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, and mercury porosimetry measurements were employed to characterize of the obtained samples. Measurements of densities and open porosities by immersion technique were used, according to the Archimedes principle. The relations between mechanical characteristics of the samples formed by using different pressures and sintered at different temperature, were discussed.     

Microstructural evolution,mechanical and thermal properties of LaB6 embedded in Si-B-C-N prepared by spark plasma sintering

Si-B-C-N monoliths with 5 wt% LaB₆ additives were prepared by spark plasma sintering at 1250–2000 °C and 50 MPa using a mechanically alloyed mixture of graphite, c-Si, h-BN and LaB₆ powders as the starting materials. Microstructural evolution, mechanical and thermal properties of the as-prepared La/Si-B-C-N monoliths were investigated. The densification of the ceramics starts at 1160° and ends at 1800 °C with the formation of La-containing compounds coupled with SiC and BN(C) phases. La-containing BN(C) grains develop into a lamellar structure at 1900 °C offering improved fracture toughness and decreased Vickers hardness, flexural strength and elastic modulus. The formation of lamellar BN(C) is also responsible for a high thermal expansion coefficient of 4.2×10⁻⁶ /°C.     

Development of crystalline phases in sintered glass-ceramics from residual E-glass fibres

The crystalline phase evolution during firing of glass-ceramic materials from residual E-glass fibres was investigated as a function of temperature and time. The thermal stability and the mechanism of crystallisation were studied by differential scanning calorimetry (DSC). The mineralogical and microstructural characterisation of the sintered glass-ceramics was carried out by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM), respectively. The crystallisation behaviour was depicted by the TTT (Time–Temperature–Transformation) curve. The activation energies for crystallisation were calculated by the Friedman differential isoconversional, ASTM and Kissinger methods. The results show that devitrification of the glass leads to a series of glass-ceramic materials composed of wollastonite and plagioclase s.s. Their microstructure is composed of a dense network of crystals, which is responsible for the high mechanical properties exhibited by these materials.     

Sintering effect on mechanical properties of composites of natural hydroxyapatites and titanium

This study presents the fabrication and characterization of composite materials of hydroxyapatite and Ti. Hydroxyapatite (HA) powder was obtained from bovine bones (BHA) and human enamel (EHA) via calcination technique. Fine powders of HA were admixed with 5 and 10 wt.% fine powder of metallic Ti. Powder-compacts were sintered at different temperatures between 1000 and 1300 °C. Compression strength, Vickers microhardness and elastic modulus as well as density were measured. SEM and X-ray diffraction studies were also conducted. The experimental results showed that addition of Ti to EHA and BHA decreases the elastic modulus, comparing to samples of pure BHA. The best mechanical properties for BHA–Ti composites were obtained after sintering in the range of 1200–1300 °C and for EHA–Ti composites in the range of 1100–1300 °C.     

Densification and properties of lime with V2O5 additions

Sintering of lime was carried out in the presence of V₂O₅ by a single firing process. A pure limestone was crushed, mixed with 1, 2 and 4 wt.% V₂O₅, pelletised and fired between 1550 and 1650 °C. The sintered lime was evaluated by bulk density, apparent porosity, microstructure, hydration resistance and hot modulus of rupture (HMOR) at 1300 °C. Incorporation of V₂O₅ forms liquid phase with lime at elevated temperature and influences the densification process by liquid phase sintering. As a result bulk density of sinters improved and they become more hydration resistant due to the larger grain size of the lime phase. The hot strength increased up to a certain temperature followed by deterioration because of the pressure of higher amount of liquid phase.     

Sintering of a clay from Burkina Faso by dilatometry Influence of the applied load and the pre-sintering heating rate

The sintering of a pottery clay from Burkina Faso was studied as a function of the heating rate, at 3 or 10°C/min. The experimental method used was loading dilatometry in isothermal conditions at 1120°C. In these conditions, we found that the densification rate of the material is low, but tend to a limiting value after 2 h at 1120°C, depending on the pre-sintering heating rate and the load used. The relationship between the pre-sintering heating rate and the densification rate indicated the existence of a weakly organised material at higher heating rates. Nevertheless, higher values of shrinkage were observed when the temperature increased continuously. It is, therefore, proposed that the material is subject to a preferential solid state diffusion mechanism at face to face of the remaining kaolinite layers at high temperatures. This mechanism is favoured by higher heating rates, mainly in the temperature range corresponding to the structural reorganisation of the metakaolin phase.