Synthesis of basic aluminum sulfate assisted by microwave heating

The synthesis of basic aluminum sulfate (BAS) was promoted by the microwave heating of a mixture of aluminum sulfate, aluminum nitrate, and sodium hydroxide. The heating process was facilitated by microwaves set at different temperatures and reaction time durations. The obtained products were characterized by X-ray diffraction and scanning electronic microscopy. Crystallographic and morphological analysis revealed BAS, boehmite, or a mixture of both products, depending on the reaction conditions.     

Preparation of coatings on alumina ceramic for wettability

To improve the wetting ability between ceramic and metal, titanium and copper coatings on alumina ceramics were prepared by infiltration of molten salt and electroless plating, respectively. A Ti/Cu bi-layer was also obtained by combining the two methods. The preparation process was optimized. The phase composition of the coatings was analyzed by X-ray diffraction (XRD). And the wettability of the titanium coating was investigated. The results showed that the copper droplet was easily spread on the surface of titanium coated alumina. The titanium coated alumina was well composited with high chromium white cast iron and the interface between ceramic and metal was well combined.     

Optimization of binder removal for ceramic microfabrication via polymer co-extrusion

The objective of this study is to assess the feasibility of solvent extraction (SE) for partial binder removal in the context of polymer co-extrusion with a thermoplastic binder component. Polymer co-extrusion is able to produce multilayered, functionally graded and/or textured structures in an efficient manufacturing process, but requires a polymer binder system with suitable flow characteristics. Traditionally, the binder is removed by thermal debinding (TD), which, however, is prone to form cracks or blisters, both of which are attributed to a lack of initial pore space that allows pyrolysis products to escape. The primary focus of this work is to demonstrate that a binder system with a high soluble binder content is suitable for conventional polymer co-extrusion and to document that a two-step binder removal process involving both SE and TD eliminates debinding defects. The overall fabrication process is documented for the extrusion of solid ceramic rods and co-extrusion of tubes, where alumina powder was batched with polyethylene butyl acrylate (PEBA) as backbone polymer and polyethylene glycol (PEG) as water soluble binder. SE for specimen with varying PEBA:PEG ratios was tested in water at three different temperatures for various times. The 1:1 mixture showed a PEG removal up to 80 wt.% of the original PEG content after 6 h extraction; after subsequent thermal debinding, rods and tubes sintered successfully without defects, demonstrating the viability of the process.     

Sintering of Al2O3-SiC composite from sol-gel method with MgO, TiO2 and Y2O3 addition

Al₂O₃-SiC composite ceramics were prepared by pressureless sintering with and without the addition of MgO, TiO₂ and Y₂O₃ as sintering aids. The effects of these compositional variables on final density and hardness were investigated. In the present article at first α-Al₂O₃ and β-SiC nano powders have been synthesized by sol-gel method separately by using AlCl₃, TEOS and saccharose as precursors. Pressureless sintering was carried out in nitrogen atmosphere at 1600 °C and 1630 °C. The addition of 5 vol.% SiC to Al₂O₃ hindered densification. In contrast, the addition of nano MgO and nano TiO₂ to Al₂O₃-5 vol.% SiC composites improved densification but Y₂O₃ did not have positive effect on sintering. Maximum density (97%) was achieved at 1630 °C. Vickers hardness was 17.7 GPa after sintering at 1630 °C. SEM revealed that the SiC particles were well distributed throughout the composite microstructures. The precursors and the resultant powders were characterized by XRD, STA and SEM.     

Effect of Y2O3 additive on conventional and microwave sintering of mullite

Mullite has become a strong candidate material for advanced structural and functional ceramics. Much interest has recently focused on sintering aids for mullite. The aim of this study was to evaluate the effect of Y₂O₃ as a sintering aid in the conventional and microwave sintering of mullite. To accomplish this study, a highly pure industrial mullite was used. Mullite with and without Y₂O₃ was pressed under a cold isostatic pressure of 200 MPa. Samples were sintered conventionally at 1400, 1450, 1500, 1550 and 1600 °C for 2 h and microwave-sintered for up to 40 min using a large range of power. The microstructure and physical properties of the microwave-sintered samples were compared to those of the conventionally sintered samples. The results showed that Y₂O₃ improved the densification of mullite bodies in the conventional and microwave sintering processes, but high densifications were achieved in just a few minutes when Y₂O₃ was used with microwave processing.     

Influence of corrosion and mechanical loads on advanced ceramic components

Advanced oxide ceramics are prospective materials for severe application conditions, including corrosion, particularly, in oxygen-rich environments, combined with the action of mechanical loads. The corrosion behavior and mechanical strength decrease of oxide ceramics, such as high alumina, alumina–mullite and zirconia-based ceramics, were studied in water steam supercritical conditions (elevated temperatures and pressures). The strength decrease under the action of the studied aggressive environment is mostly dealt with the glassy phase dissolution and intergranular corrosion for alumina–mullite and high alumina ceramics, while degradation of zirconia-based ceramics is also dealt with the phase transformation. The influence of structure defects related to processing of the ceramics on corrosion is considered.     

The role of zircon particle size distribution, surface area and contamination on the properties of silica-zircon ceramic materials

Zircon is used as an additive to silica ceramics for use in investment casting to improve their high temperature properties. However, little is known about the mechanisms by which this occurs. To investigate the effect of zircon addition to a silica ceramic a number of silica-zircon formulations were created utilising three different batches of zircon with different particle size distributions (PSDs), surface areas and contaminant inclusions. The contaminant inclusion of the zircon, present in the zircon from the ball-milling stage of manufacture, appeared to have a large effect on the room temperature flexural strength, high temperature flexural strength and high temperature creep properties. It is also suggested that any increase in post-fired cristobalite content and any change to crystal growth morphology was due to the inherent contaminant inclusions and not because of the zircon itself. Hence, use of silica-zircon materials in ceramics for investment casting should account for variation in the contaminant inclusion of the zircon in order to maintain the specific material properties required.     

Sintering of aluminum nitride by using alumina crucible and MoSi2 heating element at temperatures of 1650 °C and 1700 °C

Aluminum nitride (AlN) ceramics, prepared with Y₂O₃ and CaO sintering additives, have been densified in an Al₂O₃ crucible at temperatures of up to 1650 °C and 1700 °C using a conventional MoSi₂ heating element furnace. The results of this study show that relative densities in excess of 99% of theoretical and a relatively high-thermal conductivity of 147 W m⁻¹ K⁻¹ have been achieved for feedstock materials prepared with combined addition of 1 wt.% Y₂O₃ and 1 wt.% CaO. All of the phases in sintered samples have been shown to be crystalline AlN and minor amount of secondary phases, were detected such as enriched Y- and Ca-aluminates by the XRD patterns, back-scattered imagery and microprobe analysis. The advantage of using the particular experimental system and sintering condition is considered to be amenable to lower production cost and enhance the feasibility of mass production. Critical temperature for AlN densification to obtain the highest density is about 1650 °C.     

OH and COOH functionalized single walled carbon nanotubes-reinforced alumina ceramic nanocomposites

Alumina ceramics reinforced with 1 wt.% single-walled carbon nanotube (SWCNT) were fabricated via spark plasma sintering (SPS) of composite powders containing carboxyl (COOH) or hydroxyl (OH) group functionalized single-walled carbon nanotubes. The samples were SPS’ed at 1600 °C under 50 MPa pressure for holding time of 5 min and at a heating rate of 4 °C/s. The effects of CNT addition having different surface functional groups on microstructure, conductivity, density and hardness were reported. It was shown that nanotube addition decreased the grain sizeof alumina from 3.17 μm to 2.11 μm for COOH-SWCNT reinforcement and to 2.28 μm for COOH-SWCNT reinforcement. The hardness values of the composites are similar for all samples but there is 4.5 and 7.5 times increase in electrical conductivity with respect to monolithic alumina for COOH-SWCNT and OH-SWCNT, respectively. It was also shown by TEM and FEG SEM observations that transgranular fracture behaviour of alumina was changed to mostly intergranular fracture mode by the addition of both types of CNTs which may be due to location of CNTs along the grain boundaries. A significant grain size reduction in alumina is considered toresult fromthe suppressing effect of CNTs during sintering.     

Development of input output relationships for self-healing Al2O3/SiC ceramic composites with Y2O3 additive using design of experiments

Al₂O₃/SiC ceramic composites with Y₂O₃ as an additive, was synthesized using the Taguchi method of design of experiments, so as to develop statistically sound input output relationships. The proportion of SiC was varied from 12 to 21 vol.% whereas that of Y₂O₃ was varied from 2.5 to 4 vol.%. The composites were sintered at 1500 °C for a soaking time period of 12 h in an air atmosphere. Cracks were induced on the composite surface using a Vickers indenter with a load varying between 20 and 40 kg. Fractographical analyses have been carried out using optical and/or scanning electron microscopy to investigate the surface crack propagation behavior. Thermal aging at 1300 °C in the time range of 0.5-12.5 h was applied to find optimal conditions for healing of the pre-cracked samples. The output parameters such as crack length, healed crack length, hardness and fracture toughness of the samples were correlated with appropriate inputs such as contents of SiC and Y₂O₃, crack-healing temperature, healing time, compaction pressure, indentation load using statistical analysis. Further, the extent of influence, exerted by pertinent input parameters on output parameters, was also identified.     

Consolidation of nanoparticle suspensions by centrifugation in non-porous moulds

Alumina and zirconia nanosuspensions with a mean particle size of 100 nm and 15 nm, respectively, were consolidated by centrifugal compaction in non-porous moulds. The nanosuspensions consolidated by high-speed centrifugation were deposited irregularly, resulting in a powder deposit with density profile. The homogeneity of the powder deposits was described and homogeneous and well packed deposit regions were identified. Plate-like bodies were prepared from the homogeneous regions of the deposit. The advantage of regular and dense nanoparticle packing by centrifugal compaction was demonstrated by fabricating transparent alumina and tetragonal zirconia ceramics. The transparent alumina had an in-line transmission of 55% in the visible light at a thickness of 0.8 mm. The transparent tetragonal zirconia reached a dense microstructure with an average grain size of 65 nm and an in-line transmission of 25% at a thickness of 0.5 mm.     

Hydration of CAC cement in a castable refractory matrix containing processing additives

A growing demand for refractory castables with a particular behavior has been inducing a continuous technological evolution, where one of the most important aspects, is an in-depth knowledge of hydraulic binders. These materials greatly influence the rheological properties and mechanical strength evolution of castables, defining their workability range and demolding time, respectively. The hydration process of hydraulic binders is influenced by the presence of matrix and additives (dispersants and accelerators), which affect the setting and demolding time of shaped bodies. In this work, the influence of these variables on the hydration process of calcium aluminate cement was studied by means of temperature measurements, oscillatory rheometry and normal force measurement. These techniques were able to evaluate the setting behavior of different binders, either in plain water or in matrix-representative suspensions. In both cases, the dispersants presented a retarding effect on the hydration process, which was more significant for citric acid and diammonium citrate. The combination of these additives with an accelerator (Li₂CO₃) was shown to be an efficient tool to control the setting time of castables.     

Influence of magnesia on sintering stress of alumina

The sintering stress and the densification of MgO-doped Al₂O₃ were measured with a self-loading apparatus and a thermomechanical analyzer, respectively. The densification started at 950 °C and finished at about 1450 °C. The measured surface tensions were 0.7–0.8 N m⁻¹ in the intermediate sintering stage but drastically decreased to 0.2 N m⁻¹ in the final stage of sintering.     

Castable matrix,additives and their role on hydraulic binder hydration

The influence of alumina-based castable matrices, dispersants and Li₂CO₃ on the hydration process of different hydraulic binders was evaluated. The experiments were followed by temperature measurements with the time, the oscillatory rheometry technique and the normal force during the penetration of a blade through the material’s surface. By doing these tests, the chemical features of binder hydration, working and demolding time of suspensions could be assessed. The experiments have shown that the alumina-based matrix presented an accelerating effect which is related to its sodium content. Citric acid and ammonium citrate were the dispersants with the highest delaying effect and could be effectively associated with the accelerator (Li₂CO₃) in order to adjust the setting time of the suspensions. Nonetheless, their accelerating and retarding effect varied according to the hydraulic binder.     

A new direct coagulation casting process for alumina slurries prepared using poly(acrylate) dispersant

Direct coagulation casting (DCC) of concentrated aqueous alumina slurries prepared using ammonium poly(acrylate) dispersant has been studied using MgO as coagulating agent. Addition of small amounts of MgO increased the viscosity of the concentrated alumina slurries with time and finally transformed it in to a stiff gel. Sufficient working time for degassing and casting could be achieved by cooling the slurries to a temperature of ∼5 °C after proper homogenization after the addition of MgO. The DCC slip with alumina loading in the range of 50–55 vol% showed relatively low viscosity (0.12–0.36 Pa s at shear rate of 93 s⁻¹) and yield stress (1.96–10.56 Pa) values. The wet coagulated bodies prepared from slurries of alumina loading in the range of 50–55 vol% had enough compressive strength (45–211 kPa) for handling during mould removal and further drying. The coagulated bodies prepared from slurries of alumina loading in the range of 50–55 vol% showed linear shrinkage in the range of 4.8–2.3 during drying and 17.1–16.2 during sintering respectively. Near-net-shape alumina components with density >98% TD could be prepared by the DCC process.     

Rheological characterization of a gelcasting system based on epoxy resin

The in situ polymerization of an aqueous system comprising epoxy resin and polyamine has been developed to consolidate ceramic suspensions in our previous study. In the present work, the polymerization of the aqueous solution was investigated by an oscillatory method in terms of storage modulus G′. The influences of the epoxy resin on alumina suspensions were evaluated by means of zeta potential and viscosity. The consolidation behaviors of suspensions with different solids were also studied.     

Investigation on mechanochemical synthesis of Al2O3/BN nanocomposite by aluminothermic reaction

Alpha-alumina–boron nitride (α-Al₂O₃–BN) nanocomposite was synthesized using mixtures of aluminum nitride, boron oxide and pure aluminum as raw materials via mechanochemical process under a low pressure of nitrogen gas (0.5 MPa). The phase transformation and structural evaluation during mechanochemical process were investigated by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and differential thermal analysis (DTA) techniques. The results indicated that high exothermic reaction of Al–B₂O₃ systems under the nitrogen pressure produced alumina, aluminum nitride (AlN), and aluminum oxynitride (Al₅O₆N) depending on the Al value and milling time, but no trace of boron nitride (BN) phases could be identified. On the other hand, AlN addition as a solid nitrogen source was effective in fabricating in-situ BN phase after 4 h milling process. In Al–B₂O₃–AlN system, the aluminothermic reaction provided sufficient heat for activating reaction between B₂O₃ and AlN to form BN compound. DTA analysis results showed that by increasing the activation time to 3 h, the temperature of both thermite and synthesis reactions significantly decreased and occurred as a one-step reaction. SEM and TEM observations confirmed that the range of particle size was within 100 nm.     

Sintering behavior of nano alumina powder shaped by pressure filtration

In the present study, the sintering behavior of a commercial nano alumina powder with an initial particle size of 100 nm was investigated. The shrinkage response of the powder formed by pressure filtration (PF) during non-isothermal sintering was measured in a laser assisted dilatometer at three different heating rates of 2, 10 and 25 °C min⁻¹ up to 1400 °C. In order to calculate the activation energy of sintering, constant rate of heating (CRH) was employed and the activation energy was found to be 608 ± 20 kJ mol⁻¹ for iso-density method. The heating rate was demonstrated to have a vital role on densification behavior and final grain size. The mean grain size of the full dense specimens decreased from 875 to 443 nm when the heating rate increased from 2 to 25 °C min⁻¹.