Micro powder injection moulding of alumina micro-channel part

A feedstock consisting of submicron alumina powder and a formulated binder, was developed to fabricate alumina micro-channel part by micro powder injection moulding. During small scale-mixing, the mixing torques of feedstocks with four different powder loadings were used to establish a suitable powder loading. The thermal and rheological properties of the selected feedstock were examined and used to establish conditions for large scale mixing, debinding and injection moulding. The micro-channel parts were pressureless sintered at different temperatures. The results showed that the moulded, debound and sintered micro-channel parts had good shape retention. The dimensions of the micro-channel part changed with the different processing steps. High densification of the micro-channel parts was achieved at sintering temperatures of 1350 °C and above. Above 1350 °C, the grain grew significantly with increasing the sintering temperatures and thus it led to a decrease in the microhardness.     

Microstructural development of interface layers between co-sintered alumina and spinel compacts

Tests were performed to investigate the microstructure of the interface between alumina and spinel materials after high temperature thermal treatment (1500 °C). The first test involved co-sintering of co-pressed alumina and spinel compacts. Microstructures were investigated by SEM, EDS, WDS and EBSD. A microstructurally distinct layer with columnar grains of up to 40 μm length and 5 μm width was observed after 16 h at 1500 °C. Growth rate of the columnar spinel grains from parent spinel towards alumina follows parabolic kinetics, controlled by a mixed process of O²⁻ ion diffusion and interface reaction. Diffusion couples of spinel and alumina were investigated. Same columnar spinel grains were observed at the interface which grew into alumina during thermal treatment with the same kinetics as in co-sintering experiments. The shape of the phase boundaries between spinel and alumina can be a further indication of the direction of their growth.     

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.     

Sliding wear behaviour of alumina/nickel nanocomposites processed by a conventional sintering route

The wear resistance of Al₂O₃/2.5 vol.% Ni nanocomposites sintered by a conventional route was studied under ball-on-disk dry sliding conditions and compared with the same nanocomposites but consolidated by spark plasma sintering, together with alumina obtained by the same technique and by hot pressing. The results showed an improvement of about 0.5, 1 and 2 orders of magnitude, respectively. Thus, alumina/Ni nanocomposites processed by conventional route can compete, in cost and wear performance, with nanomaterials obtained by more sophisticated techniques.     

A study in the mechanical milling of alumina powder

The mechanical milling of alumina in order to reduce grain sizes to ≤100 nm has been proposed as a means of reducing sintering temperatures and improving pressureless sintered density, particularly as a means of allowing co-firing with metallic components for biomedical implants. There is a persistent problem with contamination from the milling media, usually hardened steel which can be only partially alleviated by acid leaching. We have explored the use of alternative milling media with a view to reducing the levels of contamination. Alumina powders were milled with hardened steel, tungsten carbide, alumina and zirconia milling media under identical conditions of ball mass:powder mass ratio 10:1 and target milling times of 32 h. All of the milling media were found to cause unacceptable levels of contamination. Zirconia media gave the lowest contamination (3–4%) and in some circumstances, the addition of a small amount of zirconia may lead to increased toughness without loss of bio-compatibility.     

Production of highly aligned porous alumina ceramics by extruding frozen alumina/camphene body

We herein propose a new technique for producing highly aligned porous ceramics by extruding a frozen ceramic/camphene body. To accomplish this, an alumina/camphene slurry with an initial alumina content of 10 vol% was first frozen unidirectionally in a 20 mm × 20 mm mold and extruded through a reduction die with a cross-section of 5 mm × 5 mm at room-temperature. This simple process enabled the formation of porous alumina ceramics with highly aligned pores as a replica of the camphene dendrites with a preferential orientation parallel to the extrusion direction. The sample showed much higher compressive strength of 280 ± 80 kPa with a porosity of 83 vol% when tested parallel to the direction of pore alignment. In addition, these materials could be used as a valuable framework for the production of ceramic/epoxy composites, particularly with a lamellar structure, which would result in a remarkable increase in mechanical properties.     

Effect of the volume ratio of zirconia and alumina on the mechanical properties of fibrous zirconia/alumina bi-phase composites prepared by co-extrusion

Fibrous zirconia/alumina composites with different composition were fabricated by piston co-extrusion. After a 3rd extrusion step and sintering at 1600 °C, crack-free composites with a fibre width of 50 μm were obtained for all compositions. The effect of the volume ratio of secondary phase on the mechanical properties was investigated. The Young's modulus of the composites decreased linearly with increasing the zirconia content. The fracture toughness of the composites was improved by introducing fine second phase filaments into the matrix. The maximum fracture toughness of 6.2 MPa m^1/2 was attained in the 3rd co-extruded 47/53 vol% zirconia/alumina composite. The improvement in toughness was attributed to both “stress-induced” transformation of zirconia and a crack deflection mechanism due to thermal expansion mismatch between the two phases. Bending strength of the composites was almost the same as that of the monolithic alumina regardless of the composition.     

In situ vibration enhanced pressure slip casting of submicrometer alumina powders

This paper presents a novel method for improvement of particle packing in consolidation of submicrometer alumina powders by pressure slip casting. In this method, filtration cell is subjected to a mechanical vibration field with constant frequency of 50 Hz and vibration amplitudes ranging from 0 (no vibration) to 2 mm. Filtration rate, thickness and green density of the fabricated samples were measured to investigate the influence of vibration on filtration characteristics. It was revealed that employment of vibration can significantly increase filtration rate. Furthermore, there is an optimum vibration amplitude which results in the structure with the highest packing density. This value is shifted to higher vibration amplitudes as more concentrated alumina slurries is used. As the available formulation based on Darcy's law could not predict the results of the present investigation, a “Correction Factor” was utilized in order to increase the accuracy of the prediction in the presence of a vibration field.     

High strain rate indentation-induced deformation in alumina ceramics measured by Cr fluorescence mapping

Alumina materials with a range of grain sizes and purities were subjected to small-scale dynamic impact by sharpened tungsten carbide projectiles at sub-ballistic velocities. The resistance of the materials to fracture was recorded by visual examination of the cracking on the impacted surface and the damage in the subsurface region. The residual stress and plastic deformation induced in each material were examined using Cr³⁺ fluorescence mapping. A modified Hertzian indentation model of the stress state in the material with the addition of a blister field representing the stress induced by the presence of the subsurface plastic zone was found accurately describe the observed cracks beneath the surface of the material, as well as the radial cracks on the surface.     

Microstructure and mechanical properties of alumina ceramics reinforced by boron nitride nanotubes

Boron nitride nanotubes (BNNTs)/alumina composites were fabricated by hot pressing. The mechanical properties of the composites are greatly dependent upon the content of BNNTs. In comparison with monolithic alumina, the incorporation of BNNTs results in the improvement of bending strength and fracture toughness owing to the effective inhibition of grain growth. A routine toughening mechanism, especially the bridging of BNNTs at grain boundaries and the sufficient physical bonding between BNNTs and alumina matrix, is dominantly responsible for the increase in mechanical properties.     

Influence of green state processes on the sintering behaviour and the subsequent optical properties of spark plasma sintered alumina

The present investigation gives a quantitative correlation between different green microstructures, and their sintering behaviour during spark plasma sintering. The green microstructures were elaborated via various green shaping processes such as direct casting and direct coagulation casting compared to uniaxial compaction of the as-received sub-micron grained corundum powder. Narrowing pore size distribution and reducing pore size (≈40 nm) in the green compact could favour cold densification during initial uniaxial pressing by grain sliding and rearrangement. This is attributed to the soft homogeneous touching network in direct-cast green samples. Consequently, grain growth was impeded and the onset of shrinkage was delayed. Moreover, the small pores and the narrow pore size distribution in the homogeneous green bodies led to higher final densities, with better optical properties compared to the less homogeneous green samples.     

Effect of freeze-drying treatment on the optical properties of SPS-sintered alumina

This study looks at the influence of alumina powder processing on the preparation of transparent alumina by Spark Plasma Sintering (SPS). Zeta potential measurements were carried out on alumina suspensions in order to determine the best dispersion conditions. Stable slurries were submitted to a spray freeze drying process and their sintering behavior was compared with the corresponding non spray freeze dried powders. Transparent alumina samples were successfully prepared from alumina powders by Spark Plasma Sintering. An optical model considering pore and grain size distributions has been developed to obtain information about porosity in dense materials. It was found that the final density and, accordingly, the optical properties were improved when spray freeze dried starting powder was used.     

Effect of alumina on the structure and properties of polyimide matrix films

To improve the properties of polyimide (PI), different mass fractions of alumina (Al₂O₃) nanoparticles, unmodified or modified by KH550, were incorporated into PI matrix to form PI/Al₂O₃ hybrid films by in situ polymerisation. The effects of Al₂O₃ additives on the structure, dielectric and mechanical properties of the films were studied. Fourier transform infrared spectroscopy confirmed the successful preparation of PI/Al₂O₃ hybrid films, and the microstructures of the samples showed a more uniform dispersion of the modified Al₂O₃ nanoparticles than the unmodified ones in the matrix. The dielectric constant of the films increased with increasing filler content, and the maximum electrical breakdown strength of 311 MV m^?1 was obtained with a filler content of 8.0 wt-% modified Al₂O₃ in the matrix. Both unmodified and modified Al₂O₃-reinforced PI hybrids demonstrated improved mechanical properties compared with the PI matrix. Moreover, the properties of films with Al₂O₃ modified by KH550 were better.     

Defect and microstructural evolution during drying of soapnut-based alumina foams

The present study demonstrates the use of soapnut, a naturally occurring surfactant for producing alumina ceramic foams. A range of slurry compositions with soapnut amounts ranging from 2 to 20 wt% in water, alumina loading of 35–55 vol% were studied. Though all slurry compositions foamed when subjected to mechanical agitation the formation of green ceramic foams free of macroscopic defects was found to be strongly dependent on conditions during drying of foamed slurries. Addition of guar gum to the slurries was shown to enhance foam stability and thus produce defect-free foams from compositions that otherwise either collapsed or resulted in other macroscopic defects during drying. Drying conditions also had a strong effect on microstructural parameters such as cell size and cell connectivity. Soapnut-based foams appear to have a greater connectivity between cells than foams produced by other comparable processes.     

Taguchi design of experiments approach to the manufacture of one-step alumina microfilter/membrane supports by the centrifugal casting technique

The Taguchi design of experiments method was implemented for the optimization of the manufacture of sintered one-step alumina microfilter/membrane supports by the centrifugal casting technique for the first time. A 10 wt.% alumina aqueous slip containing Tiron (0.001 g/g alumina) as dispersant and PVA as binder were used. Acceleration (3 levels), slip volume (3 levels), binder content (3 levels) and pH (2 levels) were selected as controlling parameters (saturated L-9 array). The use of three different target functions has been discussed: (1) the product of top-layer surface porosity times the reciprocal of top-layer surface pore diameter; (2) the product of permeability times thickness; and (3) membrane curvature. It is deduced that the first target function is the most appropriate as far as the membrane characteristics of the sintered compact are concerned. Using this target function a distinct optimum configuration for the controlling parameter levels could be obtained.     

Effects of the nature of the doping salt and of the thermal pre-treatment and sintering temperature on Spark Plasma Sintering of transparent alumina

A slurry of α-Al₂O₃ was doped with Mg, Zr and La nitrates or chlorides, in various amounts in the range 150-500 wt ppm and then freeze-dried to produce nanosized doped powder (∼150 nm). The powder was sintered by SPS to yield transparent polycrystalline alpha alumina. The influence of the nature of the doping element and the starting salt, the thermal treatment before sintering and the sintering temperature on the transparency of the ceramics were investigated. The transparency of the ceramics of nanosized Al₂O₃ was shown to depend mainly on the way the powder was prepared, the nature of the doping salt also had an effect. Finally, a high real inline transmittance, reaching 48.1% was achieved after optimization.     

Effect of varied powder processing routes on the stabilizing performance and coordination type of polyacrylate in alumina suspensions

The influence of initial pH and energy input during suspension homogenization on the stabilizing performance and coordination type of commercial available polyacrylate dispersant were studied. Additionally to widely used rheology and electroacoustic measurement techniques the alumina suspensions were analysed with centrifugal separation and in situ ATR-FTIR to study the impact of varied powder processing in detail. In contrast to zeta potential analysis and viscosity measurements only the determination of sedimentation properties by centrifugal separation shows the effect of macroscopic changes in powder processing. A combination of positively charged alumina surface and a high shear homogenization leads to the most stable suspension. Accordingly ATR-FTIR results show a correlation between improved suspension stability and inner-sphere coordination of polyacrylate. Moreover it was possible to determine an optimal pH range for inner-sphere adsorption. It can be shown that macroscopic changes in powder processing influence the coordination of dispersant and thus the suspension stability.     

Microstructural design and elaboration of multiphase ultra-fine ceramics

Three-phase composites in the system Al₂O₃-YAG-ZrO₂ (AYZ) were produced by doping the surface of commercial alumina nanopowders with inorganic precursors of the second phases. Materials with three different compositions were prepared, in which 5, 20 and 33 vol.% of each second phase were respectively present. Pure crystalline phases were obtained in the final composites, as assessed by X-ray diffraction. Green bodies were produced by slip casting and uniaxial pressing. Subsequent free sintering led to full densification and to highly homogeneous microstructures, in terms of grain size and second phase distribution. A progressive refinement of the alumina matrix grain size was achieved by increasing the second phase content, varying from micro/nano-composites to ultra-fine structures, with a mean grain size of about 500 nm for all the phases. The three materials presented high Vickers hardness values, as a results of the high final density and ultra-fine, homogeneous microstructures.     

High temperature mechanical characterisation of an alumina refractory concrete for Blast Furnace main trough: Part I. General context

Blast Furnace main trough is an industrial structure submitted to severe high temperature cyclic loading applied on its inner lining made of refractory concrete. The attempt to increase the lifetime of such a structure by numerical simulation requires a proper experimental characterisation of all materials involved and particularly of the refractory concrete. The present paper exposes an analysis of the conditions required for an experimental setup in accountancy with the material working conditions. Then, the development of a performing high temperature mechanical testing device aimed at characterising the castable behaviour in its service conditions is introduced. In particular an original extensometer allowing high temperature direct measurement of the specimen height variation has been developed. Lastly, results of an uniaxiale compression test carried out at intermediate temperature are presented and discussed.     

Evaluation of sintering stresses of an Al2O3 powder with a self-loading apparatus

The sintering stress of an Al₂O₃ powder, σ_s, is evaluated from an equation σ_s = F_s/ρS_a, where F_s is the uniaxial tensile force necessary to just stop the sintering contraction, ρ is the relative density, and S_a is the cross-sectional area. During densification, σ_s increases to the maximum at a relative density of 85%, and then abruptly decreases. The variation of σ_s in the intermediate sintering stage suggests a simple cubic packing of particles. Densification in the final sintering stage is explained by shrinkage of the pores at the corners where four tetrakaidecahedra meet. The present surface tensions of the Al₂O₃ powder evaluated from the σ_s roughly equal a reported value.