Effect of temperature and heating rate on the sintering of leucite-based dental porcelains

The aim of this work was to determine the effect of temperature and heating rate on the densification of four leucite-based dental porcelains: two low-fusion (Dentsply-Ceramco and Ivoclar) and two high-fusion commercial porcelains (Dentsply-Ceramco). Porcelain powders were characterized by differential thermal analysis (DTA), X-ray diffraction (XRD), particle size distribution, helium picnometry, and by scanning electron microscopy. Test specimens were sintered from 600 to 1050 °C, with heating rates of 55 °C/min and 10 °C/min. The bulk density of the specimens was measured by the Archimedes method in water, and microstructures of fracture surfaces were analyzed by scanning electron microscopy (SEM). The results showed that densification of specimens increased with the increase in temperature. The increase in the heating rate had no effect on the densification of the porcelains studied. Both high-fusion materials and one of the low-fusing porcelains reached the maximum densification at a temperature that was 50 °C lower than that recommended by the manufactures.     

Glass–ceramic frits for porcelain stoneware bodies: Effects on sintering,phase composition and technological properties

In the present work, the effects of glass–ceramic frits (10 wt.%) added to a porcelain stoneware body in replacement of non-plastic raw materials were evaluated simulating the tile-making process. Each glass–ceramic frit plays its own peculiar effect on the compositional properties and only some precursors behave as real glass–ceramic materials. The positive influence of glass–ceramic precursors in promoting the sintering stands out when temperature onset densification and sintering rate are considered: both of them are improved with respect to the reference body. The presence of glass–ceramic frits allows to preserve good technological properties, complying with the latest requirements of the industrial practice.     

Isothermal sintering of barium-zinc-titanate ceramics

Mixtures of BaCO₃-ZnO-TiO₂ were mechanically activated using high-energy planetary ball mill during 20, 40 and 80 min. As the time of mechanical activation increased, the decrease in particle size was observed. The effect of milling on microstructure was investigated by scanning electron microscopy, as well. Sintering process was performed in air at 1100 and 1200 °C for 2 h. Various phases are present within mixtures sintered at 1100 and 1200 °C, and almost pure BaZn₂Ti₄O₁₁ phase was obtained after 80 min of milling and sintering at 1200 °C for 2 h.     

Effect of sintering temperature on microstructure and mechanical properties of zirconia-toughened alumina machinable dental ceramics

This study investigated the effect of sintering temperature on the microstructure and mechanical properties of dental zirconia-toughened alumina (ZTA) machinable ceramics. Six groups of gelcast ZTA ceramic samples sintered at temperatures between 1100 °C and 1450 °C were prepared. The microstructure was investigated by mercury intrusion porosimetry (MIP), X-ray diffraction (XRD), and scanning electron microscopy (SEM) techniques. The mechanical properties were characterized by flexural strength, fracture toughness, Vickers hardness, and machinability. Overall, with increasing temperature, the relative density, flexural strength, fracture toughness, and Vickers hardness values increased and more tetragonal ZrO₂ transformed into monoclinic ZrO₂; on the other hand, the porosity and pore size decreased. Significantly lower brittleness indexes were observed in groups sintered below 1300 °C, and the lowest values were observed at 1200 °C. The highest flexural strength and fracture toughness of ceramics reached 348.27 MPa and 5.23 MPa m^1/2 when sintered at 1450 °C, respectively. By considering the various properties of gelcast ZTA that varied with the sintering temperature, the optimal temperature for excellent machinability was determined to be approximately 1200–1250 °C, and in this range, a low brittleness index and moderate strength of 0.74–1.19 µm^−1/2 and 46.89–120.15 MPa, respectively, were realized.     

The sintering kinetics of porcelain bodies made from waste glass and fly ash

Porcelain is a material produced from kaoline, quartz and potassium-feldspar. Recently, research of new materials, for example non-hazardous wastes, that are able to replace traditional fluxing agents without changing the process or quality of the final products has been realized. The aim of this work is to study the possibility of the use of glass powder waste and fly ash together for manufacturing porcelain. Instead of quartz, fly ash was used at the selected porcelain composition. The waste glass was added partially and fully in replacement of potassium-feldspar. Samples were fired in an electric furnace with a heating rate of 10 °C/min at 1100, 1150 and 1200 °C for a period of 1, 2, 3 and 5 h. The sintered samples were characterised by XRD (X-ray diffraction) and SEM (scanning electron microscopy). Sintering activation energies were determined based on the bulk density result. At 10, 15, 20 and 25 wt.% glass waste addition, the apparent activation energies were calculated to be 145, 113.5, 70.4 and 53.74 kJ/mol, respectively. It was found that the sintering activation energy decreased with increasing waste glass addition.     

The effect of Al2O3 on sintering and crystallization of MgSiO3-based glass-powder compacts

The influence of Al₂O₃ (8 wt.%) on sintering and crystallization features of glass powders based on magnesium silicate (MgSiO₃) was experimentally determined. The investigated compositions were Y_0.125Mg_0.875Si_0.875B_0.125O₃ and Y_0.125Mg_0.725Ba_0.15Si_0.875B_0.125O₃. For the experiments, glasses in bulk and frit forms were produced by melting in Pt-crucible at 1600 °C for 1.5 h. Glass-powder compacts were sintered at different temperatures between 900 °C and 1100 °C. The evolution of crystalline regime was determined by in situ recording of X-ray diffractograms of fine glass powders at elevated temperatures. The results and their discussion showed that addition of 8 wt.% Al₂O₃ in glass batches affected the thermal properties of the glasses and resulted in MgSiO₃-based glass ceramics well sintered between 900 °C and 1100 °C. In the BaO-free MgSiO₃ glass ceramics, clino- and orthoenstatite crystallize while the presence of BaO favours the formation of hexacelsian.     

Effects of the sintering atmosphere on Nb-based dielectrics

The effects of a forming atmosphere on the stability, the sintering and the dielectric properties of Ba₅Nb₄O₁₅, BaNb₂O₆, ZnNb₂O₆ and Zn₃Nb₂O₈ ceramics were investigated, because of the primary importance of the sintering atmosphere in relation to copper sintering. These Nb-based materials were sintered in air and in Ar/H₂10%. Zn-containing samples are very sensitive to the reductive atmosphere. ZnO volatilises at 800–850 °C and the resulting compound does not exhibit the expected properties. BaNb₂O₆ and Ba₅Nb₄O₁₅ are more stable in term of relative weight loss. Nevertheless, the phase analysis reveals a modification of the BaNb₂O₆ phase, what induces the degradation of the dielectric property stability versus temperature. The properties of Ba₅Nb₄O₁₅ are not modified by a sintering in reductive atmosphere. A relative permittivity of 38.8, a permittivity temperature coefficient of −150 ppm °C⁻¹ and an insulating resistivity of 10^10.9 Ω cm were obtained for this latter.     

Effect of iron oxide coloring agent on the sintering behavior of dental yttria-stabilized zirconia

To explore the use of yttria-stabilized zirconia (YSZ) for applications in dentistry, the effect of iron oxide coloring agent on the sintering behavior of YSZ is investigated. Through the use of a small amount of iron nitrate, the color of YSZ can be tailored. The iron nitrate starts to decompose to result in iron oxide, then to dissolve into zirconia grains before the shrinkage is even started. The iron solutes enhance the sintering activity of zirconia in terms of the temperatures at the start of shrinkage and at the maximum shrinkage rate. However, the size of zirconia grains is also increased along with Fe content. More monoclinic phase is found in the specimens with higher Fe content. The formation of m-phase is detrimental to both hardness and toughness of zirconia, limiting the amount of coloring agent can be added.     

Evaluation of aluminosilicate glass sintering during differential scanning calorimetry

The aim of this work is to investigate a difference in heat flow observed in the differential scanning calorimetry curves when aluminosilicate glasses are analyzed. Glasses with nominal composition 56.21 SiO₂ 18.65 Al₂O₃ 25.14 MgO (wt%) were produced by the conventional melting process. Glass frits were milled and sieved in the range of 45–63 µm. The material was analyzed by X-ray fluorescence spectrometry, X-ray diffraction, differential scanning calorimetry (DSC), and differential thermal analyses (DTA). The particle size distribution was determined by laser diffraction technique. The microstructures of the samples were observed by scanning electron microscopy after removing them from the DSC sample holder. The density was determined by He picnometry. The difference in heat flow in the DSC curves is assigned to the sintering process occurring during the heating cycle, which was confirmed by the neck formation in the particle interface, DSC signal variation in isothermal measurements, no change in the heat flow when monolith specimen are analyzed, and in subsequent DSC analysis after cooling. The concurrent crystallization was also determined.     

Characterization of submicrometer-sized NiZn ferrite prepared by spark plasma sintering

High-density submicrometer-sized Ni_0.5Zn_0.5Fe₂O₄ ferrite ceramics were prepared by spark plasma sintering in conjunction with sufficient high energy ball milling. They were evaluated by different characterization techniques such as X-ray diffraction, scanning electron microscopy, and dielectric and magnetic measurements. All samples prepared at sintering temperatures ranging from 850 to 925 °C exhibit a single spinel phase and their relative densities and grain sizes range from 90% to 99% and ~100 nm to ~300 nm, respectively. The dielectric constant increases with decreasing grain size until ~250 nm, and then decreases dramatically with further decreasing grain size. The saturation magnetization increases continuously with increasing grain size/density but the magnetic coercivity decreases. The highest dielectric constant and saturation magnetization at room temperature are approximately 1.0×10⁵ and 84.4 emu/g, respectively, while the lowest magnetic coercivity is only around 15 Oe. These outstanding properties may be associated with high density and uniform microstructure created by spark plasma sintering. Therefore, the spark plasma sintering is a promising technique for fabricating high-quality NiZn ferrites with high saturation magnetization and low coercivity.     

Synthesis of dense NiZn ferrites by spark plasma sintering

Dense NiZn ferrites were fabricated by spark plasma sintering (SPS) at 900 °C and 20 MPa in short periods. The powder was densified to 98% of the theoretical density by the SPS process. The SPS disks exhibited a higher saturation magnetization (Ms), up to 272 emu/cm³, than did the disks sintered by the conventional process. A higher coercivity (Hci) was obtained when the green bodies were sintered by the SPS process for 5 min. A modest holding time is essential to obtain fine grain and uniformity in the SPS process. Secondary crystallization, inhomogeneous microstructure and intragranular pores were found as a result of the rapid sintering and relatively longer holding time in the SPS process. Infrared (IR) spectra were also measured in the range from 350 to 700 cm⁻¹ to study the efforts of the SPS process on NiZn ferrites.     

Lightweight glass–ceramic tiles from the sintering of mining tailings

Modern thermally-insulating building façades comprise lightweight structural panels, in turn mostly composed of porcelain stoneware with engineered porosity. Sintered glass–ceramics may represent a valid alternative, mainly considering layered articles, with a dense surface layer on a highly porous body that could be manufactured by double pressing. In this paper we present a low cost route to lightweight tiles, developed starting from mining tailings, such as waste from the mining of boron-rich minerals and basalt rock, and recycled glasses, such as common soda-lime glass and pharmaceutical borosilicate glass. A highly porous body was obtained by direct sintering of mixtures of mining tailings and soda-lime glass; despite the homogeneity of porosity and the formation of new crystal phases (at only 1000 °C), favorable to good mechanical properties, the water absorption remained far above the limits (>2 wt%). The water absorption was minimized by introduction of a dense glaze, associated to the firing of mixtures coated by a thin layer of recycled borosilicate glass powders; both color and shrinkage were optimized by the mixing of borosilicate glass with powders of zircon mineral and vitrified boron waste/basalt/soda-lime mixture.     

Effects of microwave sintering on the properties of porous hydroxyapatite scaffolds

Microwave sintering was used to process porous hydroxyapatite scaffolds fabricated by the extrusion deposition technique. The effects of microwave sintering on the microstructure, phase composition, degradation, compressive strength and biological properties of the scaffolds were investigated. After rapid sintering, scaffolds with controlled structure, high densification and fine grains were obtained. A significant increase in mechanical strength was observed relative to conventional sintering. The scaffolds (55–60% porosity) microwave sintered at 1200 °C for 30 min exhibited the highest average compressive strength (45.57 MPa). The degradation was determined by immersing the scaffolds in physiological saline and monitoring the Ca²⁺concentration. The results indicated that the microwave-sintered scaffolds possessed higher solubility than conventionally sintered scaffolds, as it released more Ca²⁺ at the same temperature. Furthermore, an in vitro MC3T3-E1 cell culturing study showed significant cell adhesion, distribution, and proliferation in the microwave-sintered scaffolds. These results confirm that microwave sintering has a positive effect on the properties of porous hydroxyapatite scaffolds for bone tissue engineering applications.     

Normal sintering of (K, Na)NbO3-based lead-free piezoelectric ceramics

Lead-free piezoelectric ceramics have received more attention due to the environmental protection of the earth. (K, Na)NbO₃-based ceramics are one of the most promising candidates. Normal sintering of un-doped and Li/Ta co-doped (K, Na)NbO₃ ceramics was investigated to clarify the optimal sintering condition for densification, microstructure and electrical properties. It was found that density increased greatly within a narrow temperature range but turned to decrease when the sintering temperature slightly exceeded the optimal one. Piezoelectric properties also showed similar relationship between the density and sintering temperature, but the highest piezoelectric strain coefficients were obtained at the temperatures lower than that for the highest density. The grain growth and property change as a function of sintering temperature were discussed on basis of the formation of liquid-phase and the composition deviation caused by the volatilization of alkali components during sintering.     

Development and characterisation of triaxial electrical porcelains from Ugandan ceramic minerals

Ten formulations of triaxial porcelain composed from 30–60% clay, 20–45% feldspar and 20–25% sand, were prepared from raw materials sourced from Ugandan deposits. Specimens were made using the plastic extrusion method and characterized in terms of constituent oxide composition, flexural strength, fracture toughness, dielectric strength, microstructure and phase properties using ICP-AES analyses, 4-point load strength test, Vicker's indentation, FEG-SEM and powder-XRD analyses, respectively. XRD studies revealed that the crystalline phases are mullite and quartz and their intensity is almost identical for all samples fired at 1250 °C but there is a decrease in quartz content as temperature is increased. Samples with 20% sand content resulted in higher density, modulus of rupture and fracture toughness compared to those containing 25% sand. The major factor influencing bending strength was found to be porosity in samples as opposed to crystallinity. A sample with 67.3% SiO₂, 20.2% Al₂O₃, 3.4% K₂O and 6.3% others exhibited best properties.     

Effects of sintering temperature and holding time on porosity and shrinkage of glass tubes

The influences of sintering temperature and holding time on porosity and shrinkage of glass tubes have been studied by optical microscope. It is evident that there exists three stages for the sintering process of glass. At the first stage, both increasing temperature and prolonging the holding time contribute to lowering the porosity and to intensifying the shrinkage greatly. At the second stage, the glass further densifies and the voids among particles become smaller and less. Finally, at the third stage the shrinkage rate almost keeps unchanged to sintering temperature and holding time.     

The effect of the wet-milling process on sintering temperature and the amount of additive of SiAlON ceramics

In this study, nano-sized SiAlON powders were produced by wet milling at elevated speeds as a top-to-bottom process. Before the milling process, different milling times and mediums were performed for the determination of the most efficient milling system. The milled powders were characterized by BET and X-ray diffraction (XRD) measurements and the results were compared to standard samples. The standard powders were produced using a conventional process (the ball to powder ratio was 1:1.5, at 300 rpm, for 1.5 h) having a few hundred nanometer particle size. The nano powders were milled using a wet-milling process in an optimum medium so that the particle size was decreased down to ≈70 nm. The samples, produced from the nano powders, were densified at 150 °C lower degrees than the sintering temperature of samples which were produced by a conventional method (185 nm). However, the phase transformation of α → β-SiAlON was also observed related to the amount of additives. This transformation affected the mechanical properties of the SiAlON ceramic. The results were discussed using the relationship between density, phase composition, microstructure and mechanical properties.     

Effect of CeO2 on the sintering behaviour of zirconia–alumina composite

Precursor for a composite containing equimolar proportion of ZrO₂ and Al₂O₃ having higher reactivity has been synthesized by the wet interaction of inorganic salts in aqueous phase. Sintering of the compact body indicated that the densification rate increased from 1500 °C. The role of CeO₂ as a dopant was positive with respect to densification and retention of t-ZrO₂.     

Wear resistant boron carbide compacts produced by pressureless sintering

Boron carbide compacts were produced by pressureless sintering at 2200 °C/2 h and 2250 °C/2 h in Ar atmosphere, using a starting powder with a particle size smaller than 3 µm. Effects of carbon addition (3.5 wt%) and methanol washing of the starting powder were investigated on the densification, Vickers hardness, and micro-abrasive wear resistance of the samples. The removal of oxide phases by methanol washing allowed the production, with no sintering additive, of highly densified (93.6% of theoretical density), hard (25.4 GPa), and highly wear resistant (wear coefficient =2.9×10^–14 m³/N.m) boron carbide compacts sintered at 2250 °C. This optimized combination of properties was a consequence of a reduced grain growth without the deleterious effects associated to the carbon addition. Methanol washing of the starting powder is a simple and general approach to produce, without additives, high quality, wear resistant boron carbide compacts by pressureless sintering.     

Characterization of basaltic tuffs and their applications for the production of ceramic and glass–ceramic materials

Alkaline basaltic tuffs, from Southern Turkey were characterized and employed to obtain ceramic and glass–ceramic materials by combined sintering and crystallization process. The chemical and mineralogical compositions were analyzed by X-ray fluorescence spectrometry and X-ray diffraction analyses, respectively. The phase formation and the sintering behaviour were investigated by DTA, differential dilatometer and hot-stage microscopy. The micro-structure and residual porosity of the sintered samples were observed by SEM and evaluated by pycnometric techniques. Ceramic material, based on 50% basaltic tuff and 50% clay, was obtained at 1150 °C with 13% total porosity and 4% water absorption. Glass–ceramic materials were synthesized directly using the milled basaltic tuff by mean of the sinter-crystallization technique, in the range 900–1150 °C. The investigation has showed that, due to the high porosity and low crystallinity, alkaline tuffs could be a suitable raw material for ceramic application.