Laser shock processing of polycrystalline alumina ceramics

Laser shock processing (LSP) has been applied to polycrystalline α‐Al₂O₃ ceramics. X‐ray characterizations have revealed that LSP results in significant compressive residual stresses which can extend to a depth of more than 1.2 mm from the surface. The presence of compressive residual stresses improves the resistance of α‐Al₂O₃ ceramics to indentation cracking. Microstructural characterization suggests that the majority of α‐Al₂O₃ grains on the surface remains intact after LSP. However, damaged regions are occasionally present, which shows intergranular fractures and a limited plastic deformation in the vicinity of grain boundaries.     

Transparent alumina by vacuum sintering

Alumina windows transparent in IR range and translucent in UV range were obtained by high vacuum sintering (～10^–6 mbar). To determine the influence of the atmosphere on grain growth, a sintering kinetics and intragranular porosity studies have been performed for samples sintered in air and in high vacuum atmospheres. It has been established that by using high vacuum sintering instead of the conventional one in air, alumina compacts with lower grain size, less impurities in grain boundaries and less quantity of intragranular pores were obtained. It has been proven that high vacuum sintering allows to reach high densities (>99%th) without exaggerated grain growth (d₅₀ < 1 μm). Finally, strong correlation between microstructure and light transparency has been found and consequently it can be concluded that vacuum sintering clearly enhances the optical properties of alumina.     

Dense mullite zirconia composites obtained from the reaction sintering of milled stoichiometric alumina zircon mixtures by SPS

The main objective of this article is to obtain dense (porosity under 0.5%) polyphasic ceramics belonging to the Al₂O₃–SiO₂–ZrO₂ system by SPS sintering of high energy powders milled drily; the stoichiometric (54.45:45.54 zircon–alumina, weight basis) mixture was explored in this work. Particularly the principal sintering variables: sintering temperature and dwell time were investigated. The textural, structural and microstructural changes were evaluated together with the hardness and toughness of the obtained ceramics and their microstructure. The effect of the mechanical pre-treatment was carried out by X-ray diffraction and particle distribution evaluation. Due to the rapid heating process an incomplete reaction was achieved in several cases, as a consequence multiphasic ceramics with different alumina, mullite, zircon and zirconia contents were obtained.     

Carbon nanotube/boehmite-derived alumina ceramics obtained by hydrothermal synthesis and spark plasma sintering (SPS)

Preparation, structure and properties of hydrothermally treated carbon nanotube/boehmite (CNT/γ-AlOOH) and densification with spark plasma sintering of Al₂O₃ and CNT/Al₂O₃ nanocomposites were investigated. Hydrothermal synthesis was employed to produce CNT/boehmite from an aluminum acetate (Al(OH)(C₂H₃O₂)₂) and multiwall-CNTs mixture (200 °C/2 h.). TEM observations revealed that the size of the cubic shape boehmite particles lies around 40 nm and the presence of the interaction between surface functionalized CNTs and boehmite particles acts to form ‘nanocomposite particles’. Al₂O₃ and CNT/Al₂O₃ compact bodies were formed by means of spark plasma sintering (SPS) at 1600 °C for 5 min using an applied pressure of 50MPa resulting in the formation of stable α-Al₂O₃ phase and CNT–alumina compacts with nearly full density. It was also found that CNTs tend to locate along the alumina grain boundaries and therefore inhibit the grain coarsening and cause inter-granular fracture mode. The DC conductivity measurements reveal that the DC conductivity of CNT/Al₂O₃ is 10^?4 S/m which indicate that there is a 4 orders of magnitude increase in conductivity compared to monolithic Al₂O₃. The results of the microhardness tests indicate a slight increase in hardness for CNT/Al₂O₃ (28.35 GPa for Al₂O₃ and 28.57 GPa for CNT/Al₂O₃).     

Transparent polycrystalline alumina using spark plasma sintering: Effect of Mg,Y and La doping

Transparent polycrystalline alumina (PCA) is a promising replacement for sapphire. Its optical properties however are highly dependent on the grain size and residual porosity which need to be controlled for real inline transmittances (RIT), that are high enough for possible applications.To achieve high RITs, doping as well as pressure assisted sintering is often used. In this study spark plasma sintering (SPS) and doping are investigated. A systematic experimental design is used to study the influence of Mg, Y and La single or co-doping (75–450 ppm) as well as the SPS sintering pressure and temperature on the RIT and grain size of PCA.Using optimized sintering parameters, RITs of >50% were attained in the visible wavelength (640 nm) for 0.8 mm thick samples for almost all doping strategies. The best RIT of 57% was for triple-doped samples at a total dopant level of 450 ppm. These results are significantly better than previously published SPS studies and illustrate that SPS sintered alumina can attain high and reproducible optical transmittances under various doping and sintering conditions.     

Densification of alumina by SPS and HP: A comparative study

In this study, the densification of alumina by spark plasma sintering (SPS) was investigated and compared to conventional hot pressing. It was shown that SPS is very effective in the sintering of alumina leading to higher densities and allows to work at lower temperatures and with shorter sintering cycles. The effect of the heating rate is dependent on the heating mode (SPS or HP). The identification of active sintering mechanisms was attempted by an isothermal and an anisothermal methods, showing that other mechanisms probably related to electrical effects enhance the densification. We suggest the higher contribution of surface diffusion mainly during the initial stage of sintering and an influence of the presence of impurities segregated at the grain boundaries. They could create conductive layers and also introduce ions with a lower valence than Al³⁺; defects are created in the surface layers and the diffusion of the species is increased.     

Creep behaviour of alumina/YAG nanocomposites obtained by a colloidal processing route

The high temperature creep behaviour (1200–1400 °C and 30–250 MPa) of high-purity alumina (A) and an alumina/YAG nanocomposite (AY) prepared by using a colloidal processing route has been studied. Creep parameters were correlated with microstructural features in order to determine the dominant creep mechanisms in both materials.It was found that the creep rate value of AY was 1 order of magnitude lower than the one of undoped alumina A. The creep mechanism for AY was found to be lattice diffusion (Nabarro–Herring) compared to a combination of grain boundary (Coble) and lattice diffusion for A. When the slow crack growth region of both materials was compared, a significant improvement was observed, i.e. the slow crack growth region of alumina shifted to nearly 2.5 times the stresses applied for AY at the temperatures of 1200, 1300 and 1400 °C.     

Transparent alumina ceramics: Effect of standard and plasma generated stabilizing approaches in colloidal processing

The study is focused on an optimization of the slip-casting process used for the fabrication of the transparent/translucent alumina ceramics; more precisely, on specifying the most appropriate way to stabilize the cast alumina suspensions. An innovative method of the particles’ stabilization by plasma treatment was compared with the classical electrostatic and the most frequently used electrosteric approach. Properties of green bodies (pore size distribution, density) and sintered samples (density, mean grain size, real in-line transmittance) were measured in term to evaluate the impact of the individual stabilization mechanism on the final properties of the transparent/translucent ceramics. The results showed that all tested approaches enable the preparation of the transparent/translucent alumina ceramics by Hot Isostatic Pressing. Ceramics prepared from the plasma treated as well as the electrostatically stabilized powders exhibited narrower pore size distribution, higher density, and lower mean grain size in comparison to ceramics fabricated from only electrosterically stabilized powders. Despite these promising properties the plasma-treated samples resulted in an unexpectedly low RIT of 36% caused by the presence of thin cracks. However, the electrostatically stabilized samples achieved the highest RIT value of 57%.     

溶胶--凝胶法制备多晶氧化铝纤维的研究

本文探讨了溶胶－凝胶法制备多晶氧化铝过程中影响体性能的因素,成纤方法与工艺参数,热处理工艺制度及晶相转移关系等一系列问题。实验得到了以莫来石为主晶相长期使用温度超过１６００℃的多晶氧化铝纤维。     

Synthesis and Densification of Transparent Magnesium Aluminate Spinel by SPS Processing

Mixtures of elementary oxides, MgO–Al₂O₃, were used to fabricate transparent polycrystalline magnesium aluminate spinel specimens by means of the spark plasma sintering technique. A sintering aid, 1 wt% of LiF, was added to the mixed powder. The presence of the additive promotes the synthesis of spinel that starts at 900°C and is completed at 1100°C. The LiF additive wets spinel on its melting and promotes densification, which is completed at 1600°C. LiF vapor plays a cardinal role in eliminating residual carbon contamination and in the fully dense state, allows attaining a 78% level of optical transmittance. The optimal conditions for achieving adequate transparency were determined and the role of the LiF addition in the various stages of the process is discussed.     

Strong pinning effect of alumina/nanodiamond composites obtained by pulsed electric current sintering

A small fraction (5 vol.%) of detonation nanodiamonds, or DND, acts as a remarkably effective boundary pinning agent in alumina throughout a wide sintering temperature range (from 1200 up to 1700 °C). This is the first time that such a strong grain growth inhibitory effect is observed for any of the alumina based composites of similar characteristics reported in the literature. These nanocomposites were consolidated by pulsed electric current sintering (PECS) and present bending strength (550 MPa) and toughness (5.2 MPa m^1/2) values significantly higher than the ones corresponding to alumina compacts obtained under the same sintering conditions.     

Mesoporous alumina obtained by combustion synthesis without template

Mesoporous alumina has been synthesised by the solution combustion synthesis method. While often the synthesis of mesoporous materials with a relatively narrow pore distribution requires the use of a template, this technique allows a simple and rapid synthesis of pure alumina without the use of any templating agent: by regulating the synthesis conditions is possible to obtain from relatively low surface area α-alumina to high surface mesoporous γ-alumina. The porosity of the latter was assessed chiefly by density functional method and was found to be in the range 2.8–3.5 nm. Low angle X-ray diffraction experiments demonstrated a partial ordering of the structure, with a periodicity in the range 5.5–6.9 nm. The addition of lanthanum to the alumina was tested and found to confer a good temperature resistance to the alumina, without modifying the mesoporous structure. After a prolonged heat treatment at 900 °C the mesoporosity of lanthanum-modified samples was retained, even if the pores size increased and the specific surface area decreased.     

Transparent alumina ceramics fabricated by 3D printing and vacuum sintering

Transparent alumina ceramics were fabricated using an extrusion-based 3D printer and post-processing steps including debinding, vacuum sintering, and polishing. Printable slurry recipes and 3D printing parameters were optimized to fabricate quality green bodies of varying shapes and sizes. Two-step vacuum sintering profiles were found to increase density while reducing grain size and thus improving the transparency of the sintered alumina ceramics over single-step sintering profiles. The 3D printed and two-step vacuum sintered alumina ceramics achieved greater than 99 % relative density and total transmittance values of about 70 % at 800 nm and above, which was comparable to that of conventional CIP processed alumina ceramics. This demonstrates the capability of 3D printing to compete with conventional transparent ceramic forming methods along with the additional benefit of freedom of design and production of complex shapes.     

On the fracture toughness of polycrystalline alumina measured by SEPB method

Fracture toughness (K_IC) of a polycrystalline alumina was evaluated using a single edge precracked beam (SEPB) method. A Knoop indentation-induced microcrack was introduced into a bend bar specimen, and then a sharp pop-in precrack was developed by applying the bridge loading technique. The precrack length (a/W) was varied by changing the indentation load and/or the support groove width of the anvil. The precracked specimens were fractured by three-point bending under a cross-head speed of 0·5 mm/min at room temperature. K_IC values of a polycrystalline alumina were dependent on precrack length for a/W<0·35. The dependence was discussed in terms of residual stress around the indentation-induced crack and crack mouth opening displacement (CMOD).     

Transparent high-strength nanosized yttria stabilized zirconia obtained by pressure-less sintering

This work describes the development of transparent high-strength Yttria-Stabilized Zirconia (YSZ) ceramics with ultra-fine grain size utilizing conventional pressure-less densification. Starting with nanoparticles with diameter < 10 nm, it was possible to achieve full densification (>99.5% of theoretical density) at a sintering temperature of 1100–1200 °C. The average grain size of the resulting dense ceramics was 75 nm in 3 mol. % YSZ and 85 nm in 8 mol. % YSZ, showing in-line light transmission of 38% and 51% at a wavelength of 800 nm and average biaxial strength (piston on three balls test on samples of diameter 12 mm and thickness 1 mm) of 1980 MPa and 680 MPa, respectively. The nano-grained structure, absence of color centers, and miniaturization of residual pores enable the excellent light transmission. The high biaxial strength is attributed to the refined microstructure, but also to the martensitic tetragonal-to-monoclinic phase transformation that remains active even in nano-sized zirconia grains.     

Effect of grain boundary state and grain size on the microstructure and mechanical properties of alumina obtained by SPS: A case of the amorphous layer on particle surface

The work was aimed at the investigation of kinetics of Spark Plasma Sintering (SPS) of the α-Al₂O₃ particles with amorphous surface layers and investigation of the effect of the amorphous layers on the grain growth and on the mechanical properties of alumina. The objects of investigations comprised:(i) submicron α-Al₂O₃ powder, (ii) submicron α-Al₂O₃ powder with the amorphous layers on the particles' surfaces, and (iii) the fine-grained α-Al₂O₃ powder. The submicron powders (i) and (ii) were used to analyze the effect of the amorphous layers on the sintering kinetics. Powders (i) and (iii) were used to analyze the effect of the initial particle sizes on the shrinkage kinetics. The effect of the temperature regime and of the rate (V_h) on the shrinkage kinetics of the submicron and fine alumina powders has been studied. The shrinkage curves were analyzed using the Young–Cutler and Coble models. The sintering kinetics was shown to be determined by the intensity of grain boundary diffusion for the submicron powders and by simultaneous lattice diffusion and grain boundary one for the fine powders. The amorphous layers on the surfaces of the submicron α-Al₂O₃ particles were found to affect the grain boundary migration rate and the Coble equation parameters at the final stages of SPS. The abnormal characteristics of the alumina ceramics sintered from the submicron powder with the amorphous layers on the particles’ surfaces were suggested to originate from the increased concentration of the defects and of the excess free volume at the grain boundaries formed during crystallization of the amorphous layers.     

Transparent polycrystalline MgO ceramic fabricated by low-temperature vacuum sintering with MgF2 additive

This study introduces transparent MgO ceramics produced via simply vacuum sintering at 1200–1500 °C by optimal incorporation of MgF₂ as a sintering additive. The effect of MgF₂ content and sintering temperature on the densification process, optical, and thermal properties of MgO ceramics is presented with emphasis on its function as a sintering aid and adverse effect of MgF₂ evaporation in the condition of high MgF₂ content or high sintering temperature. MgO ceramic with 1.0 mol% MgF₂ sintered at 1300 °C exhibits the highest relative density of 99.95% with average grain size of 17.46 μm. The in-line transmittance attains 60% at 1000 nm and >80% in the infrared range (3.8–6.8 μm), without absorption bands originated from the carbon contamination. The corresponding room-temperature thermal conductivity reaches 47.25 W/(m∙K). These results demonstrate that MgF₂ is an outstanding sintering additive for the preparation transparent MgO ceramics.     

Densification of SiC by colloidal processing and SPS without sintering additives

Abstract

Silicon carbide is one of the most important ceramics used as structural and functional materials in a wide variety of applications. Many studies have reported the densification of SiC using oxide and nonoxide additives such as the Al₂O₃, B₄C and Al–B–C system. However, it is difficult to densify SiC at temperatures below 2000°C without sintering additives even if spark plasma sintering (SPS) is used. The authors attempted to densify SiC using colloidal processing and SPS without sintering additives. A commercially available SiC powder with the average particle size of 0·55 μm was used as the starting material. The densities of the green body prepared by slip casting and the sintered body by SPS were 65·5 and 98·7% respectively.     

Copper tracks processing on alumina by laser cladding: Elaboration and characterization

A laser process allows achieving in air electrical tracks on alumina substrates with an electrical conductivity of 5.10⁶ S m^?1. Copper paste was first put on alumina substrates and it was heated following a narrow track (c.a. 400 μm wide). Copper melted and oxidized partially during treatment forming cuprite Cu₂O. A reaction occurs between Cu₂O and alumina substrates which provides, after cooling, a good bonding of the copper-based tracks onto the substrates. Conditions of laser exposure have to be sharply controlled: if insufficient, tracks do not adhere to the substrate, and if too long, alumina substrates are hollowed, cracked, with vaporizations of copper and ejections of alumina. However the feasibility of such a process is now established.     

Densification of transparent yttrium aluminum garnet (YAG) by SPS processing

Nano-size YAG powder co-mixed with 0.25 wt.% LiF was used to fabricate transparent polycrystalline YAG specimens by means of the Spark Plasma Sintering (SPS) technique. The presence of the LiF additive in the initial nano-powder allows obtaining fully dense disc shaped (up to 4 mm thick) transparent specimens at the outcome of a 2 h treatment at 1300 °C. The presence of LiF plays a key role in the mass transport related effects during the densification of YAG to full density and also in the elimination of the residual carbon contamination, allowing reaching a level of optical transmittance close to the theoretical value.