Starch consolidation of alumina: Fabrication and mechanical properties

A consolidation technique based on gelling property of starch was used to prepare alumina ceramics. Slurry containing alumina powder, dispersant and small amount of starch (2–3.5 wt.% of powder weight) was cast into a nonporous mould and heated to gelation temperature to produce a rigid green body. A defect free green body was obtained and the total linear shrinkage during drying was 2–3% and the green density observed was 64% of theoretical value. After complete drying, ceramic compacts were sintered without debinding operation. Sintered density of 99.4% was achieved after sintering at 1600 °C for 2 h. Flexural strength values of dried and sintered alumina were ～10 and 247 MPa, respectively. The sintered ceramics showed an extremely dense microstructure.     

Pressure filtration assisted gel casting in translucent alumina ceramics fabrication

High density and homogeneous green body is important for fabricating transparent ceramics. Inspired by the improved samples’ homogeneity in slip casting, we introduced low pressure filtration to gel casting to further increase the relative density and homogeneity of the green body and to shorten the drying time. The effect of pressure filtration on drying characteristics, bulk density and porosity of the pre-sintered bodies, and the microstructure and optical transmittance of the resultant ceramics were intensively investigated. The results showed that pressure filtration can reduce the drying time by 27.3%, improve the density of the pre-sintered bodies and reduce the residual pores of the sintered ceramics. The in-line transmittance of the translucent alumina prepared by the pressure filtration assisted gel casting was 32.7% at 600?nm with a thickness of 1?mm, which is about 6% higher than that without pressure filtration. In principle, this process can be applied to fabricate any other high-performance ceramic.     

Evolution of the microstructure and mechanical properties of stereolithography formed alumina cores sintered in vacuum

Stereolithography (SL) was used to form alumina ceramic cores. The effect of sintering temperature on the microstructure and mechanical properties of the alumina ceramics are investigated, which were sintered in vacuum. The results indicate that, as the sintering temperature increased the particle size of alumina slightly increased, and the interlayer spacing first decreased and then increased. The open porosity of alumina ceramics significantly decreased as the sintering temperature in vacuum increased. The flexural strength and hardness increased as the sintering temperature increased. When sintered at 1150 °C, the flexural strength was found to be 33.7 MPa, the shrinkage was 2.3 %, 2.4 %, and 5.3 % in the X, Y, and Z directions, respectively, and the open porosity was 37.9 %. These results are similar to those found from sintering at 1280 °C in air.     

Fabrication of translucent alumina ceramics from pre-sintered bodies infiltrated with sintering additive precursor solutions

Translucent alumina ceramics were fabricated by infiltrating aqueous solutions containing sintering dopant ions (Mg²⁺/Y³⁺/La³⁺) into pre-sintered alumina compacts and sintering in H₂ atmosphere. The improved microstructural homogeneity, finer grain size and enhanced transmission properties of infiltration processed samples over those processed by conventional ball-milling method were corroborated by experimental results. Triple doping via infiltration appears to be significantly beneficial for achieving enhanced transmission (36.3% at wavelength 800 nm for sample thickness of 0.75 mm). This study indicates that infiltration technique can be used to fabricate translucent alumina ceramics with improved performance.     

Process control and optimized preparation of porous alumina ceramics by starch consolidation casting

This work concerns details of porosity and pore size control in starch consolidation casting of alumina ceramics using corn starch. In particular, the influence of the solids loading (68-78 wt.% alumina in suspensions with nominal starch contents of 20-50 vol.%) on the porosity, bulk density and shrinkage of alumina ceramics is studied. The results indicate a linear decrease of the linear shrinkage and the bulk density (and a corresponding increase in porosity) as the alumina concentration increases, with slopes that are independent of the starch content. The pore size is characterized via microscopic image analysis, the pore throat size via mercury porosimetry. Relations between the volumetric shrinkage, porosity and the volume fractions of starch and water in the suspensions are discussed, and a new concept, called “affine limit porosity” is proposed to explain the apparently paradoxical finding that the porosity increases with increasing alumina content in the suspension.     

Non-shrinkage porous ceramics by In-situ hollow sphere method based on the Kirkendall effect of Al particle

The significant shrinkage of porous ceramics after sintering has produced a number of issues with their use and development. As a result, we proposed an in-situ hollow sphere method for producing non-shrinkage alumina porous ceramics. The obtained green samples were made up of Al₂O₃ and Al powders, with pores emerging inside the materials due to the Kirkendall effect of Al particles after sintering. The expansion of hollowing particles exactly offsets the shrinkage generated by sintering throughout the process. When 50 vol. % Al powder (10 µm) is added, the linear shrinkage rate of the sample after sintering at 1500 °C can reach −3.47 %, and its apparent porosity and flexural strength are 30.69 % and 44.03 MPa, respectively. According to approximate calculations, the pores formed by the oxidation of Al powder are smaller than the initial size of Al powder. This method suggests a novel approach for producing controlled shrinkage porous ceramics.     

Preparation and characterization of porous alumina ceramics through starch consolidation casting technique

This work aims at studying the influence of thermal treatment on the microstructure, resistivity and technological properties of porous alumina ceramics prepared via starch consolidation casting (SCC) technique. Colloidal suspensions were prepared with three different contents of alumina solid loading (55, 60 and 65 mass%) and corn starch (3, 8 and 13 mass%). The sintered samples at 1400, 1500, 1600 and 1700 °C, show open porosity between 46 and 64%, depending on the starch content in the precursor suspensions and sintering temperature. The pore structures were analyzed by SEM. The effect of corn starch content on the apparent porosity, pore size distribution, linear shrinkage and electrical resistivity as well as cold crushing strength of the sintered porous alumina ceramics was also measured. These porous alumina ceramics are promising porous ceramic materials for using in a wide range of thermal, electrical and bioceramics applications as well as filters/membranes and gas burners, due to their excellent combination properties.     

Enhanced mechanical properties of 3D printed alumina ceramics by using sintering aids

Stereolithography based 3D printing provides an efficient pathway to fabricate alumina ceramics, and the exploration on the mechanical properties of 3D printed alumina ceramics is crucial to the development of 3D printing ceramic technology. However, alumina ceramics are difficult to sinter due to their high melting point. In this work, alumina ceramics were prepared via stereolithography based 3D printing technology, and the improvement in the mechanical properties was investigated based on the content, the type and the particle size of sintering aids (TiO₂, CaCO₃, and MgO). The flexural strength of the sintered ceramics increased greatly (from 139.2 MPa to 216.7 MPa) with the increase in TiO₂ content (from 0.5 wt% to 1.5 wt%), while significant anisotropy in mechanical properties (216.7 MPa in X-Z plane and 121.0 MPa in X–Y plane) was observed for the ceramics with the addition of 1.5 wt TiO₂. The shrinkage and flexural strength of the ceramics decreased with the increase in CaCO₃ content due to the formation of elongated grains, which led to the formation of large-sized residual pores in the ceramics. The addition of MgO help decrease the anisotropic differences in shrinkage and flexural strength of the sintered ceramics due to the formation of regularly shaped grains. This work provides guidance on the adjustment in flexural strength, shrinkage, and anisotropic behavior of 3D printed alumina ceramics, and provides new methods for the fabrication of 3D printed alumina ceramics with superior mechanical properties.     

Pressure-less joining of alumina ceramics by the reaction-bonded aluminum oxide (RBAO) method

The present work demonstrates a pressure-less and reliable joining technique for alumina ceramics through a reaction-bonded aluminum oxide (RBAO) method. Effective joining relies on the RBAO mechanism, in which Al particles are converted to alumina through oxidation and bond with alumina particles from the parts to be joined upon sintering. Alumina ceramics in a green state were successfully joined with the use of an Al/Al₂O₃ powder mixture as an interlayer. The oxidation behavior of the Al particles was confirmed by thermogravimetry and X-ray diffraction analyses. Joining was performed in ambient air at 1650 °C for 2 h without applying any external pressure. Microstructural observations at the joining interfaces indicated a compact joining. The joining strengths were assessed by determining the biaxial strengths at room temperature, and the joined samples exhibited no fractures at the joining interfaces. Moreover, the joints had a strength of almost 100 % when compared with those of the parent alumina ceramics.     

Low sintering shrinkage porous mullite ceramics with high strength and low thermal conductivity via foam-gelcasting

Excessive sintering shrinkage leads to severe deformation and cracking, affecting the microstructure and properties of porous ceramics. Therefore, reducing sintering shrinkage and achieving near-net-size forming is one of the effective ways to prepare high-performance porous ceramics. Herein, low-shrinkage porous mullite ceramics were prepared by foam-gelcasting using kyanite as raw material and aluminum fluoride (AlF₃) as additive, through volume expansion from phase transition and gas generated from the reaction. The effects of AlF₃ content on the shrinkage, porosity, compressive strength, and thermal conductivity of mullite-based porous ceramics were investigated. The results showed that with the increase of content, the sintering shrinkage decreased, the porosity increased, and mullite whiskers were produced. Porous mullite ceramics with 30 wt% AlF₃ content exhibited a whisker structure with the lowest shrinkage of 3.5%, porosity of 85.2%, compressive strength of 3.06 ± 0.51 MPa, and thermal conductivity of 0.23 W/(m·K) at room temperature. The temperature difference between the front and back sides of the sample reached 710°C under high temperature fire resistance test. The low sintering shrinkage preparation process effectively reduces the subsequent processing cost, which is significant for the preparation of high-performance porous ceramics.     

Effects of particle size distribution and sintering temperature on properties of alumina mold material prepared by stereolithography

Alumina mold materials prepared by stereolithography usually have considerable sintering shrinkage, and their properties related to casting have been rarely studied. In this study, alumina molds materials were prepared by stereolithography, and the effects of particle size distribution and sintering temperature on the properties of the materials were investigated. Results show that the viscosity of the slurries decreases as the fraction of fine powder increases, and the particle size distribution affects the curing behaviors slightly. Sintering shrinkage increases as the fraction of fine powder or the sintering temperature increases. Although lower sintering shrinkage can be achieved by sintering at 1350 °C or 1450 °C, the mold materials sintered at lower temperatures would continue to shrink under the service temperature of 1550 °C, and thus 1550 °C is determined as the optimal sintering temperature. As the fraction of fine powder increases, the creep resistance first increases and then decreases, and specimens prepared with 0.1 fraction of fine powder exhibit the best creep resistance with the droop distance of 4.44 ± 0.45 mm. Specimens prepared with 0.1 fraction of fine powder and sintered at 1550 °C exhibit linear shrinkage of 6.36% along the X/Y direction and 11.39% along the Z direction, and have a flexural strength of 78.15 ± 3.50 MPa and porosity of 30.12 ± 0.08%. The resulting material possesses relatively low sintering shrinkage, proper mechanical strength, porosity and high-temperature properties that meet the requirements for casting purposes.     

Influence of debinding holding time on mechanical properties of 3D-printed alumina ceramic cores

Herein, alumina green bodies are fabricated by three dimensional (3D) printing technology, then, the influence of debinding holding time under vacuum and argon on mechanical properties is systematically investigated by comparing the changes in microstructure, bulk density, open porosity, grain connection situation and flexural strength of ceramics. The flexural strength of alumina ceramics acquired the maximum values of 26.4 ± 0.7 MPa and 25.1 ± 0.5 MPa after debinding under vacuum and argon for 120 min and 180 min, respectively. However, the alumina ceramics rendered the flexural strength of 19.4 ± 0.6 MPa and 9.5 ± 0.4 MPa under vacuum and argon without extended holding time, respectively. The relatively low mechanical properties can be mainly attributed to the weak interlayer binding force, which is caused by layer-by-layer forming mode during 3D printing process and anisotropic shrinkage during the sintering process. Moreover, the alumina ceramics exhibited moderate bulk density and open porosity of 2.4 g/cm³ and 42% after the sintering process, respectively, which are mainly influenced by the microstructural evolution of alumina ceramics during thermal treatment. Also, the diffusion of gases is achieved by curing of photosensitive resin and influenced by different holding times during debinding, affecting the mechanical properties of sintered ceramics. The mechanical properties of as-sintered ceramics are suitable for the utilization of ceramic cores in the manufacturing of hollow blades.     

Preparation and properties of porous alumina with inter-locked platelets structure

Porous alumina ceramics with alumina platelets was prepared by vapor-solid reaction sintering of AlOF mesophase gas by the reaction of HF and Al₂O₃. The effect of heating treatment temperatures on porosity, the formation of inter-locked platelets structure and compressive strength of porous alumina ceramics was determined by Archimedes' method, XRD, SEM and compressive tests. The results indicated that after heating at temperatures from 1300 °C to 1600 °C, the porosity of alumina ceramics decreased from 61.6% to 48.4%. Increasing the heating treatment temperature was beneficial to form inter-locked structure between alumina platelets. The maximum compressive strength of porous ceramics with porosity of 48.4% can reach 29.8 MPa heated at 1600 °C; this strength was attributed to the strong bonding between the alumina platelets.     

Crack-reduced alumina/aluminum titanate composites additive manufactured by laser powder bed fusion of black TiO2−x doped alumina granules

Laser powder bed fusion is an emerging industrial technology, especially for metal and polymer applications. However, its implementation for oxide ceramics remains challenging due to low thermal shock resistance, weak densification and low light absorptance in the visible or near-infrared range. In this work, a solution to increase the powder absorptance and to reduce cracking during laser processing of alumina parts is given. This is achieved by the use of a homogeneously dispersed and reduced titanium oxide additive (TiO_2?x) within spray-dried alumina granules leading to formation of aluminum titanate with improved thermal shock behavior during powder bed fusion. The impact of different reduction temperatures on powder bed density, flowability, light absorption and grain growth of these granules is evaluated. Crack-reduced parts with a density of 96.5%, a compressive strength of 346.6 MPa and a Young's modulus of 90.2 GPa could be manufactured using powders containing 50 mol% (43.4 vol%) TiO_2?x.     

Effect of particle size distribution of alumina on strength of glass-infiltrated alumina

Glass-infiltrated alumina composites were prepared by infiltrating glass into a pre-sintered alumina. Three different alumina preforms were obtained from various combinations of fine and coarse alumina particles. After infiltration of glass into the porous alumina preforms, their microstructure and strength were studied. The highest bending strength of 510 MPa was observed when the composite was made by mixing coarse and fine alumina powders at a ratio of 6:4. The infiltrated glass corroded the alumina preform, and the dissolved aluminum ions reprecipitated on the alumina grains during the heat-treatment for infiltration.     

Effect of crystallographic orientation on transparency of alumina prepared using magnetic alignment and SPS

Transparent polycrystalline alumina was developed over many years because its attractive properties are expected to find applications in many fields. Crystallographic orientation is one of the effective ways to improve transparency in birefringent ceramics such as alumina, because birefringence at grain boundaries can be suppressed by the alignment of optical axis. Fabrication of high-transparency alumina with an oriented c-axis and fine microstructure can be attained by slip casting in a strong magnetic field, followed by spark plasma sintering at 1150?°C for 20?min. The real in-line transmittance of the textured alumina with a thickness of 0.80?mm was 70% at λ?=?640?nm, which was higher than that of randomly-oriented alumina. The c-axis orientation reduced the actual difference of the refractive index and suppressed remarkably the birefringence.     

Effect of the addition of polyvinylpyrrolidone as a pore-former on microstructure and mechanical strength of porous alumina ceramics

The effect of the solvent on the properties of porous alumina ceramics was studied when polyvinylpyrrolidone (PVP) was used as an organic pore-former. In particular, porous alumina ceramics were produced by dry-pressing of mixed PVP–alumina powder; the mixing of PVP and alumina powder was achieved via ball milling using water or acetone as solvent, or dry ball milling. Due to the different solubility of PVP in water and acetone, porous alumina ceramics with different pore structures and mechanical properties were obtained. Because of its cylindrical pores being aligned to some extent, the sample prepared using acetone as solvent exhibited the highest bending strength (140.2 MPa) and Young's modulus (57.4 GPa), which were 1.6 times and 3.4 times higher compared to that prepared without PVP. Moreover, the addition of PVP via wet ball milling led to more uniform dispersion of PVP in alumina, hence limiting the grain growth during sintering process and increasing the grain bonding.     

Effect of compaction on the sintering of borosilicate glass/alumina composites

The effect of initial compaction on the sintering of borosilicate glass matrix composites reinforced with 25 vol.% alumina (Al₂O₃) particles has been studied using powder compacts that were uniaxially pressed at 74, 200 and 370 MPa. The sintering behaviour of the samples heated in the temperature range 850–1150 °C was investigated by density measurement, axial and radial shrinkage measurement and microstructural observation. The density of the sintered composites increased continuously with temperature for compacts pressed at 74 MPa, while for compacts pressed at 200 and 370 MPa it reached the maximum value at 1050 °C and at higher temperatures it decreased slightly due to swelling. The results showed anisotropic shrinkage behaviour for all the samples, which exhibited an axial shrinkage higher than the radial shrinkage, and the anisotropic character increased with the initial compaction pressure.     

Optical,mechanical and fractographic response of transparent alumina ceramics on erbium doping

Alumina ceramics found their utilisation in many applications which can be further extend by attaining functional properties; in our case the transparency obtained through precise processing and photoluminescence due to erbium (Er) doping. In order to examine the optical, mechanical and fractographic response of transparent alumina on Er doping, slip casted samples containing 0–0.15 at.% of erbium nano-oxide were pre-sintered by two-step sintering regime and then hot isostatically pressed. Prepared samples exhibited fully dense submicron microstructure and corresponding high transparency (RIT up to 60%). Positive influence of doping on the Vickers hardness resulted in values up to 27 GPa (at 10 N load). Moreover, the comparison of the Vickers hardness determined at different loadings with literature data showed that the Er doped alumina is one of the hardest material in this category. The samples were characterised also in terms of fracture toughness and fractographic behaviour.     

Effect of dispersant on paste rheology in preparation of porous alumina with oriented pores by extrusion method

The effect of additives on paste rheology was investigated for preparation of porous ceramics with unidirectionally aligned cylindrical pores. Ammonium poly-carboxylic acid (APA) used as a dispersant and it was adsorbed on alumina powder surface. The adsorption isotherm of APA was fitted by Langmuir equation. The saturated monolayer adsorption was 5.9 mg/g. The apparent viscosity became a minimum at 0.8 mass % of APA corresponding to 71.2 mPa?s. This APA amount of 5.6 mg/g, is in good agreement with the observed APA amount. Since the nylon 66 fibers (0–35 vol. %) mixed with the alumina powder have a strong interaction with each other, they became twisted and agglomerated. This agglomeration increased with increasing fiber content but decreased by adding oleic acid. The pastes with added oleic acid were capable of being extruded at higher pressure. The obtained porous alumina ceramics showed highly oriented cylindrical pores parallel to the extrusion direction. The pore orientation was higher in the oleic acid added pastes than those without oleic acid. The added nylon 66 fibers are mostly converted to pores while maintaining the original shape after sintering. The pore size distribution of the obtained porous ceramics measured by mercury porosimetry method showed a peak at about 4 μm which is apparently smaller than that observed in the SEM photographs and the obtained result is considered to be corresponding to the necks formed by fiber contacts.