Preparation of high-porosity Al2O3 ceramic foams via selective laser sintering of Al2O3 poly-hollow microspheres

In this paper, high-porosity Al₂O₃ ceramic foams called Al₂O₃ PHM ceramics were fabricated through selective laser sintering (SLS) via Al₂O₃ poly-hollow microspheres (Al₂O₃ PHMs). SLS parameters were optimized by an orthogonal experiment as to be laser power = 6 W, scanning speed = 1800 mm/s, and scanning space = 0.15 mm. The effect of sintering temperature on microstructure, shrinkage, porosity, phase composition, mechanical properties and pore size distribution of Al₂O₃ PHM ceramics were investigated. When sintering temperature increased, Al₂O₃ PHM ceramics contained only Al₂O₃ phase and were gradually densified. With the raise of sintering temperature, the porosity of Al₂O₃ PHM ceramics decreased gradually from 77.09% to 72.41%, but shrinkage in H direction and compressive strength of Al₂O₃ PHM ceramics increased from 6.63% and 0.18 MPa to 13.10% and 0.72 MPa, respectively. Sintering temperature had little effect on pore size distribution of Al₂O₃ PHM ceramics, which only declined from 24.2 to 21.4 μm with the increase of sintering temperature from 1600 to 1650 °C. This method can not only directly prepare ceramic foams with complex shapes, but also control properties of ceramic foams. It provides a simple preparation method for many kinds of ceramic foams with complex structure and high porosity by using PHMs with different composition.     

Modified Al2O3-based ceramic

Translated from Steklo i Keramika, No. 1, pp. 27–29, January, 1990.     

Direct laser melting of Al2O3 ceramic paste for application in ceramic additive manufacturing

We develop the direct laser melting of ceramic paste technology for application in ceramic additive manufacturing (AM). The Al₂O₃ ceramic paste, which is a homogeneous mixture of DI-water and Al₂O₃ ceramic powders, was deposited on an Al₂O₃ substrate using free-forming extrusion (FFE), and subsequently melted by a CO₂ laser. To better control the laser melting process, the flow behavior of the laser-melted Al₂O₃ was investigated by evaluating the microstructure of the laser-melted Al₂O₃ single tracks. When the laser scanning speed increased from 1 to 3.5 mm/s at a fixed laser power, the permeation of the molten Al₂O₃ into the surrounding porous paste was reduced, resulting in the improvement of the surface uniformity of the laser-melted Al₂O₃ tracks. Through optimizing the laser scanning strategy, a fully-dense Al₂O₃ layer with smooth surface was achieved. The phase composition and density of the laser-melted Al₂O₃ layers were evaluated to study their properties. The thickness of the dense Al₂O₃ layer varied from ～90 μm to ～120 μm periodically due to the line-by-line scanning of the Gaussian laser beam. In addition, the relationship between the melting thickness and the laser scanning speed was also investigated to further improve the controllability of the laser melting process. This direct laser melting of ceramic paste technology is promising for applications in ceramic AM, such as 3D printing of ceramic components and high-temperature ceramic welding.     

Power prediction for laser engineered net shaping of Al2O3 ceramic parts

Laser-aided additive manufacturing technique is a competitive method for direct fabrication of ceramic components. However, the optimal processing parameters are difficult to find because defects are easy to generate for ceramic parts. This paper proposes a mathematical model for predicting required laser power in direct fabrication of Al₂O₃ ceramic parts by laser engineered net shaping (LENS). The laser power model, which is derived based on energy balance of one deposition layer, reveals the relationship between laser power and other process conditions, such as powder flow rate, nozzle travel speed and physical properties of deposited material. The proposed model was then verified through a fabrication experiment of several single-bead wall Al₂O₃ ceramic parts with different laser power. Experimental results indicate that the laser power predicted by the model is accurate for different processing conditions. This model provides a new yet simple method for predicting required laser power accurately during LENS processes.     

Air plasma-sprayed Y2O3 coatings for Al2O3/Al2O3 ceramic matrix composites

Al₂O₃/Al₂O₃ ceramic matrix composites (CMC) are candidate materials for hot-gas leading components of gas turbines. Since Al₂O₃/Al₂O₃ CMC are prone to hot-corrosion in combustion environments, the development of environmental barrier coatings (EBC) is mandatory. Owing to its favorable chemical stability and thermal properties, Y₂O₃ is considered a candidate EBC material for Al₂O₃/Al₂O₃ CMC. Up to 1 mm thick Y₂O₃ coatings were deposited by means of air plasma spraying (APS) on Al₂O₃/Al₂O₃ CMC with a reaction-bonded Al₂O₃ bond-coat (RBAO). APS Y₂O₃ coatings exhibit a good adherence in the as-deposited state as well as upon isothermal annealing up to 1400 °C. Moreover, furnace cyclic testing performed at 1200 °C revealed an excellent durability. This is explained by the formation of a continuous, approximately 1 μm thick reaction zone at the APS Y₂O₃/RBAO interface. The reaction zone between Y₂O₃ and Al₂O₃ comprises three layers of thermodynamically stable yttrium-aluminates exhibiting strong bonding, respectively.     

Self-lubricating behaviors of Al2O3/TiB2 ceramic tools in dry high-speed machining of hardened steel

In this paper, Al₂O₃/TiB₂ ceramic cutting tools with different TiB₂ content were produced by hot pressing. The fundamental properties of these ceramic cutting tools were examined. Dry high-speed machining tests were carried out on hardened steel. The tool wear, the cutting temperature, the cutting forces, and the friction coefficient between the tool and the chip were measured. It was shown that both the wear rates and the friction coefficient at the tool–chip interface of Al₂O₃/TiB₂ ceramic cutting tools in dry high-speed machining of hardened steel were reduced compared with that of in low-speed machining. The mechanisms responsible were determined to be the formation of a self-lubricating oxide film on the tool–chip interface owing to the tribological–chemical reaction by the elevated cutting temperature. The composition of the self-lubricating film was found to be the oxidation product of TiB₂ grains, which serves as lubricating additive on the wear track of the tool rake face. The appearance of this self-lubricating oxide film contributed to the improvement in wear resistance and the decrease of the friction coefficient. This action was even more effective with higher TiB₂ content. Cutting speed was found to have a profound effect on the self-lubricating behavior. In dry low-speed machining of hardened steel, the Al₂O₃/TiB₂ tools showed mainly adhesive and abrasive wear. While in dry high-speed machining, oxidation wear of the ceramic tools was the dominant mechanism due to the very high cutting temperature. No oxide film was formed on the tool–chip interface while machining in nitrogen atmosphere, and the tool wear resistance was correspondingly decreased.     

CO2 laser peeling of Al2O3 ceramic and an application for the polishing of laser cut surfaces

A laser controlled fracture peeling technique is demonstrated to smooth the Al₂O₃ ceramic surface without thermal damages. It was found that a chip can be separated and curled from the ceramic surface during a focused CO₂ continuous wave (CW) laser dual-scanning. The thickness of the curled chip is ～50 μm and the formed subsurface roughness (R_a ≈ 2 μm) is close to the surface machined by mechanical breaking (R_a = 1.84 μm). The chip formation is attributed to the controlled fracture by the residual tensile stress in the recast layer, whereas the chip curling only occurs when the melting depth is shallower than the position of lateral cracks. The peeling technique can be applied to polish the cut surface of laser fusion cutting in ceramics. The polished cut surface (R_a = 2.18 μm) is free from recast, crack and heat effects. The microstructure is similar to the base material. The material removal rate during polishing is up to 0.125 mm³/s.     

Effect of process parameters on crack characteristics in laser welding of Al2O3 ceramic

The crack of ceramic weld is a worldwide problem for brittle material, high energy laser beam is expected to solve this problem. In this paper, the crack of fiber laser welding of Al₂O₃ ceramics was studied. The weld crack rate was used to characterize the crack condition of weld, and the influences of laser power, welding speed and defocusing distance on crack characteristics were carried out. The results showed that Al₂O₃ ceramics weld has obvious crack tendency, and the cracks mainly appeared on the weld center line. When the crack appeared on the weld center line, there was crack-free on the base metal. When the defocusing distance increased from +3 mm to +20 mm, the number of cracks gradually decreased. When the defocusing distance was greater than +17 mm, cracks-free appeared on the weld and base metal. Abaqus software was used to simulate the relationship between crack and stress based on thermal elastoplastic theory. The high crack areas, few crack areas and free crack areas were divided according to the maximum principal stress value. No matter what welding conditions, as long as the maximum principal stress was less than 1576 MPa, there was crack-free on the weld and base metal.     

液相法制备棒状Al2O3及Al2O3-ZrO2陶瓷复合粉体

采用二乙三胺五乙酸（DTPA）为配合剂,以简易的液相法合成出微纳米纤维状Al和Al-Zr前体,煅烧处理制备了棒状α-Al₂O₃和Al₂O₃-ZrO₂复合陶瓷粉体。同时研究了DPTA∶Al³⁺质量比、反应温度与时间对陶瓷粉体形态的影响。利用X射线衍射（XRD）、热分析（TG/DSC）以及扫描电子显微镜（SEM）对粉体进行了表征。结果表明：较高的DTPA∶Al³⁺质量比以及较长的反应时间有利于制备高长径比的纤维棒状Al和Al-Zr配合物前体。合成纳米纤维状α-Al₂O₃和Al₂O₃-ZrO₂前体的最优条件是反应温度60℃,反应时间5.5h,DTPA∶Al³⁺比例为1.2∶1。相应地,该前体煅烧后可以制备出棒状α-Al₂O₃和Al₂O₃-ZrO₂复合陶瓷粉体。     

等离子喷涂Al2O3陶瓷涂层的研究

研究等离子喷涂Al2O3陶瓷涂层的抗热震性能,分析并计算等离子喷涂Al2O3陶瓷涂层和AlAl2O3涂层中的残余应力,得出了两种涂层的应力分布,测试了TiO2含量对Al2O3陶瓷涂层性能的影响,检验了影响涂层质量的工艺参数.     

A strong ceramic in the Al2O3-ZrO2-Y2O3 system

Conclusions A highly dense ceramic based on the eutectic composition of the Al₂O₃-ZrO₂ system was obtained using 3 mole % Y₂O₃ addition. The ceramic has a fine-grained structure and high hardness and strength.Translated from Ogneupory, No. 2, pp. 8–10, February, 1987.     

CO2 capture based on Al2O3 ceramic membrane with hydrophobic modification

In this paper, Al₂O₃ ceramic membrane is modified to hydrophobicity by grafting 1 H,1 H,2 H,2 H-perfluorodecyltriethoxysilane. And its properties are characterized in detail. CO₂ capture performance of ceramic membrane is investigated by experiments. Results show that wetting resistance after modification is significantly improved, and contact angle increases from the initial 49.8–130.9°. However, hydrophobic modification has no significant effect on the crystalline phase, surface morphology and pore size distribution of the ceramic membrane. With ethanolamine (MEA) as absorbent, CO₂ mass transfer rate and capture efficiency using modified hydrophobic ceramic membrane are 46.6 × 10⁻³ mol/(m²·s) and 98.0%, showing significantly increase compared to the original membrane. After 72 h immersion in MEA solution, quality of ceramic membrane does not change significantly. And there is almost no change in average pore size. We believe this study will provide a reference for the industrial application for CO₂ capture by gas-liquid membrane contactor with ceramic membrane.     

Microstructure and mechanical properties of Al2O3/Y3Al5O12/ZrO2 hypereutectic directionally solidified ceramic prepared by laser floating zone

Al₂O₃/Y₃Al₅O₁₂/ZrO₂ directionally solidified ceramic has been considered as a promising candidate for ultrahigh temperature structural materials due to its excellent performance even close to its melting point. In this work, laser floating zone (LFZ) solidification experiments were performed on Al₂O₃/Y₃Al₅O₁₂/ZrO₂ hypereutectic with the solidification rates between 2 μm/s and 30 μm/s. The full eutectic lamellar microstructure is obtained with hypereutectic composition. The solid/liquid interface morphology is investigated. The microstructure characteristic is discussed based on the solid/liquid interface. The variation of lamellar spacing with different compositions and solidification rates was reported and discussed by considering an irregular eutectic growth model. The maximum hardness and fracture toughness are 19.06 GPa and 3.8 MPa m^1/2, respectively. The toughening mechanism of ZrO₂ is discussed based on the scenario of the crack propagation pattern.     

CO2 laser post-treatment of sol-gel-derived Y3Al5O12:Ce phosphor ceramic powders

Cerium-doped yttrium aluminum garnet (Y₃Al₅O₁₂:Ce, YAG:Ce) was prepared using a sol-gel method and then fired for CO₂ laser post-treatments. Phase transformations and formation of impurities were not observed in YAG:Ce after CO₂ laser sintering. The shift of the diffraction peak and the appearance of another Raman peak indicate a more homogeneous distribution of Ce activators and enhanced crystallinity in laser-sintered YAG hosts. Larger spheres (100–200 μm) with tiny crystallites (<10 μm) were observed on the smoother surface in the laser-sintered YAG:Ce, unlike the irregular, porous, and layered powders in the sol-gel-derived YAG:Ce (1–100 μm). Photoluminescence (PL) measurements revealed an emission increase of 180% and a red shift of the emission peak for the laser-sintered YAG:Ce powders compared with the sol-gel-derived powders. Both have comparable thermal PL quenching behavior; however, the YAG:Ce powders with CO₂ laser treatment exhibited a PL efficiency improvement of approximately 4%.     

Near-zero-shrinkage Al2O3 ceramic foams with coral-like and hollow-sphere structures via selective laser sintering and reaction bonding

The large shrinkage that ceramics undergo during sintering is a severe challenge for high-performance porous ceramics. In this study, we report a powder-based selective laser sintering (SLS) approach to prepare Al₂O₃ ceramic foams with near-zero shrinkage, high porosity, and outstanding strength. The ceramic foams consist of specific coral-like and hollow-sphere structures derived from the raw Al₂O₃/Al composite powders via reaction bonding (RB). A near-zero shrinkage of 0.91 ± 0.15 % and a high porosity of 73.7 ± 0.2 % can be achieved based on the Kirkendall effect during the oxidation of Al particles. Meanwhile, the reinforced sintering necks and robust bond-bridge connections between hollow-sphere and coral-like structures result in a remarkable bending strength of 7.37 ± 0.37 MPa. This measured strength is more than six times higher than other fabricated samples from spherical Al₂O₃ powders, and the comprehensive performance of ceramic foams prepared by this novel SLS/RB strategy is exceptionally remarkable versus that via conventional forming methods.     

Crystallization kinetics of La2O3–Al2O3–B2O3 glass–ceramic composites

One glass formulation (L2 glass) with the composition of La₂O₃, Al₂O₃ and B₂O₃ in a molar ratio of 10:10:80 was selected to cofire with Al₂O₃ filler. The composites underwent a two-stage crystalline evolution in the temperature range of 800 to 975 °C. The crystallization kinetics of LaBO₃ grains and the transformation to LaAl₂B₃O₉ phase were investigated by DTA, XRD, SEM/EDS, and TEM. The results showed that the Al₂O₃ filler plays an important role as the heterogeneous sites of LaBO₃ nuclei, and as reactant for the formation of flaky LaAl₂B₃O₉ crystals. The apparent activation energy of LaBO₃-phase formation in L2 glass was 534 kJ/mol and reduced to 466 kJ/mol by the addition of Al₂O₃. The detail transformation reactions, kinetics, and the crystalline orientation relationship between those phases are reported.     

Incorporating sugarcane bagasse ash into Al2O3 ceramic tapes

High-temperature co-fired ceramic (HTCC) technology aims to incorporate fluxing materials into ceramic tapes to decrease the sintering temperature. In this context, we incorporate waste from sugarcane bagasse ash (SCBA) into alumina (Al₂O₃) tapes. We report an experimental investigation of the structural, physical, mechanical, and dielectric properties of the Al₂O₃ tape with the addition of the SCBA waste. The tape casting technique prepared the ceramic tape. The materials under study were characterized by rheology, thermogravimetry, dilatometry, X-ray diffraction, scanning electron microscopy, relative density, Vickers microhardness, mechanical resistance, and dielectric measurements. The dilatometry results confirm that the addition of the SCBA waste remarkably reduces the sintering temperature of the Al₂O₃ tape to 1200°C. The physical, mechanical, and dielectric properties are improved with the addition of the SCBA waste, which makes our discoveries attractive from an environmental and economic point of view. Besides, the stabilization and high dielectric constant of the Al₂O₃-SCBA tape becomes a promising material for aircraft turbine applications.     

Direct ink writing of aluminum-phosphate-bonded Al2O3 ceramic with ultra-low dimensional shrinkage

Three-dimensional (3D) printing of ceramics has attracted increasing attention in various fields. However, the pyrolysis of organic components used for binding or polymerization in 3D printing commonly causes a large shrinkage (up to 30 %–40 %), high porosity, and cracking or deformation, severely limiting practical applications. In this study, 3D printing of Al₂O₃ ceramic architectures with ultra-low shrinkage is realized by introducing inorganic binder aluminum dihydrogen phosphate (Al(H₂PO₄)₃, AP) as a ceramic precursor. Compared to organic binders, the inorganic AP binder can undergo crystallization conversion, which reduces mass loss during sintering at high temperatures, resulting in low shrinkage. Moreover, AP can be used as a rheological modifier to regulate the printability of the ceramic ink for direct ink writing of Al₂O₃ ceramic architectures, such as wood-piled scaffolds, honeycomb structures, and tubes with high fidelity. The resultant Al₂O₃ structural ceramics sintered at 1250 °C exhibit good mechanical performance and structural integrity. Most importantly, the linear shrinkage of the printed ceramics is less than 5 %, which is several times lower than that of ceramics with organic binders. This study provides a viable strategy for fabricating high-performance ceramic architectures with good dimensional fidelity for practical applications.     

Synthesis of CoAl2O4/Al2O3 nanoparticles for ceramic blue pigments

The demand for pigments for industrial ceramic ink-jet printing is increasing steadily. The main challenge is the availability of ceramic pigments comprised of small-sized particles in order to avoid clogging of the printer head nozzle. This work presents a novel way to prepare ceramic blue pigment as a shell/core structure of CoAl₂O₄/Al₂O₃ nanoparticles through a simple and low-cost process. In this process, the colour tone of nano-pigment can be tuned by the selection of the cobalt precursor/Al₂O₃ ratio and calcining temperature.