Frozen slurry-based laminated object manufacturing to fabricate porous ceramic with oriented lamellar structure

The freeze drying-based additive manufacturing can be used to process porous ceramics. However, the lack of freezing direction leads to the disorderly porous structure. This paper proposes a frozen slurry-based laminated object manufacturing (FS-LOM) for processing porous ceramics. Slurry was composed of water, alumina powder, and organic binder. The water in the fresh slurry layer crystallized to obtain a good support strength. The outline of 2D pattern was cut with laser to gasify ice crystal and binder. After stacking, the ice crystal freeze dried to obtain a porous structure. The lamellar ice crystals were induced to growth vertically by layer-by-layer freezing. The uniformity and orientation of the pore structure were improved, and the compression strength of the parts were improved. Due to the support of frozen slurry, the deformation of the green part was avoided.     

陶瓷纤维催化剂载体的制备及其性能

利用陶瓷纤维毡为原料,通过适当的成型工艺将纤维毡制备成陶瓷纤维催化剂载体.探讨浸润助剂(十二烷基硫酸钠,SDS)用量、纤维毡的干燥工艺及黏结剂浓度对陶瓷纤维催化剂载体的成型和性能的影响.确定最优的成型工艺,以质量分数0.2％的SDS作浸润助剂,150℃干燥2 min,质量分数30％的硅溶胶作黏结剂,浸渍粘结后烘干,即制...     

Permeability and thermal expansion properties of porous LAS ceramic prepared by gel-casting method

The porous lithium aluminosilicate (LAS) ceramics with controllable pore structure were fabricated by gel-casting method. The porosity, pore structure, compression strength, gas permeability, and coefficient of thermal expansion (CTE) of the porous LAS ceramics with different monomer content were investigated. The sample with 5 wt.% monomer content has maximum value of compression (26.62 ± 0.54 MPa). When the monomer content increased to 20 wt.%, the porosity, Darcian gas permeability, and thermal expansion coefficient increased to maximum (63.66 %, 13.3 × 10⁻¹³ m², and 1.1–2.6 × 10⁻⁶ K⁻¹). The non-Darcian gas permeability showed irregular variation (1.35–3.61 m) with the increase of monomer content. A thermal vibration model was induced to investigate the effect of temperature and monomer content on the CTE. The results showed that the CTE increased with the increase of temperature due to the nonlinear thermal vibration of the atoms in lattice and the asymmetry of the force between particles.     

Facile preparation of morph-genetic SiC/C porous ceramic at low temperature by processed bio-template

A porous morph-genetic SiC/C ceramic material was fabricated using biomass-derived C template, Si powder, and Fe(NO₃)₃·9H₂O as the starting materials. The effects of heating temperature, and catalyst/Si mole ratio on the formation of SiC/C ceramic were investigated. In addition, the pore size distribution was obtained through pore size analysis, and the determination of oxidation resistance of SiC/C ceramics and C template was carried out by thermogravimetric analysis. The results show that copious amounts of SiC nanowires, which were distributed on the surfaces and interiors of the C template holes, were formed at 1300 °C with 4 wt% Fe as catalyst. The SiC nanowires significantly affected the oxidation resistance and microporous structures of the prepared materials. Moreover, a possible formation mechanism for the porous SiC/C ceramic was determined.     

Densification behaviour and three-dimensional printing of Y2O3 ceramic powder by selective laser sintering

The selective laser sintering (SLS) of an yttria (Y₂O₃) ceramic powder was studied to understand both the effects of i) the initial yttria particle characteristics on the powder bed behaviour and ii) the process conditions (laser power, scanning speed, hatching space) on the sintering/melting of three-dimensionally printed objects. The roughness of the powder bed, a sensitive indicator of the layer bed quality, was determined through three-dimensional optical profilometry and the powder bed packing density was modelled using the discrete-element method. Complex shaped objects including spheres and open rings were successfully fabricated by the SLS three-dimensional printing. In addition, SLS cube-shaped samples were characterized by X-ray diffraction and scanning electron microscopy. The open pore volume fraction significantly decreased from 41% without a post-SLS heat treatment to 31% with a post-SLS heat treatment at 1750 °C for 20 h under secondary vacuum. Finally, an anisotropy in elastic properties has been highlighted, Young's modulus reaches 11 GPa in the stiffest direction.     

堇青石陶瓷蜂窝载体的微观结构分析

采用XRD、SEM、EDS以及N2和汞吸附-脱附比表面积和孔径分布等分析手段,对机动车尾气净化催化剂陶瓷蜂窝载体的微观结构进行了研究。结果表明:虽然国内产品的化学组成和相组成与国外产品的基本相同,但其比表面积和孔结构等微观结构相差较大。这主要是由于国外采用全生料配料成型,在一次烧成中同时完成堇青石的合成和产品的烧成;而国内普遍采用合成的堇青石配料,经过挤出成型、干燥、切割后再烧成,致使堇青石原料中堇青石晶粒之间的孔被压塌陷,最终产品中的孔主要是堇青石二次颗粒之间的孔。据此认为,我国应努力研究堇青石的一次合成(烧成)工艺,这既能提高产品性能又能降低能源消耗。     

Powder bed selective laser processing (sintering / melting) of Yttrium Stabilized Zirconia using carbon-based material (TiC) as absorbance enhancer

This study aimed to process 8 mol.% yttrium stabilized zirconia by powder bed selective laser processing, as well known as selective laser sintering / melting. Titanium carbide was used as absorbance enhancer to a Nd:YAG laser. Titanium carbide was chosen for having the lowest weight / absorbance ratio among four additive options: silicon carbide, carbon black, graphite, and titanium carbide. Several trials were performed using 0,25 wt.% of titanium carbide as absorbance enhancer of 8 mol.% yttrium stabilized zirconia, testing different laser powers, laser speeds, laser strategies, hatch distances and designs. A window of optimized parameters was identified within the study conditions, capable of manufacturing parts with high relative density. In addition, challenges and technical aspects are discussed by analyzing the observed phenomena.     

Asymmetric porous cordierite ceramic membranes prepared by phase inversion tape casting and their desalination performance

Asymmetric porous cordierite ceramic membranes were fabricated by phase inversion tape casting method. It is shown that the membranes consist of a relatively dense skin layer on the top, a sponge layer at the bottom and a finger-like layer in the middle. The membranes have a hierarchical pore structure, where macrovoids (denoted as dozens-micron-sized (DMS) pores) are present in the finger-like layer and micron-sized (MS) pores are located in the skin layer, sponge layer and the wall of macrovoids. After surface silylation by post-grafting with 1H,1H,2H,2H-perfluorodecyltriethoxysilane (FAS), the sample with a starting powder/polyethersulfone (PESf) weight ratio of 9 (M − 4) becomes hydrophobic, with a water contact angle of 150°. At a NaCl concentration of 3.5 wt%, a feed rate of 18L/h and a feed temperature of 80 °C, the hydrophobic M − 4 membrane exhibits a water permeate flux of 22.33 kg/m²h, which is considerably larger than that of the membranes prepared by dry pressing method previously, and a salt rejection of 99.9%. The higher water permeate flux is attributed to the much lower transport resistance of water vapor in the membranes of the present work.     

Performance optimization of Si/SiC ceramic triply periodic minimal surface structures via laser powder bed fusion

SiC ceramic lattice structures (CLSs) via additive manufacturing (AM) have been recognized as potential candidates in engineering fields owing to their various merits. Compared with traditional SiC CLSs, SiC triply periodic minimal surface (TPMS) CLSs could possess more outstanding properties, making them more promising for wider applications. Since SiC CLSs are hard to be fabricated through stereolithography techniques because of inferior light performance, the laser powder bed fusion (LPBF) process via selective sintering is an effective method to prepare near-net-shaped SiC TPMS lattices. As the mechanical performances of lattice structures are the foundation for future practical applications, it is of great significance to optimize the preparation process, thus improving the mechanical properties of SiC TPMS structures. In this work, the optimal printing parameters of the LPBF and liquid silicon infiltration process for SiC ceramic TPMS CLSs with three different volume fractions were systematically illustrated and analyzed. The effects of the printing parameters and carbon densities on the fabrication accuracy, microstructure, and mechanical performance of SiC TPMS CLSs were defined. The mechanism of the reactive sintering process for the SiC TPMS lattice structure was revealed. The results reveal that Si/SiC TPMS CLSs with optimum preparation have superior manufacturing accuracy (most less than 6%), relatively high bulk densities (about 2.75 g/cm³), low residual Si content (6.01%), and excellent mechanical properties (5.67, 15.4, and 44.0 MPa for Si/SiC TPMS CLSs with 25%, 40%, and 55% volume fractions, respectively).     

Direct ink writing additive manufacturing of porous alumina-based ceramic cores modified with nanosized MgO

Alumina-based ceramic cores, widely applied to cast alloy, have been restricted by the increased complexity of castings, the resultant complex equipment and cost. In this research, to address the aforesaid disadvantages, direct ink writing, a green additive manufacturing method, is utilized to directly fabricate a new kind of nanosized MgO strengthened alumina-based ceramic cores. Slurries with various compositions exhibits ideal shear-thinning behaviors, owing to the hydrogen bond formed between polyvinylpyrrolidone and kaolin molecules. We notice that introducing nanosized MgO reduces drying shrinkage of green specimens and greatly promotes liquid-phase sintering, leading to rather more densified samples. Overall, it is anticipated that the current approach is effective in rapidly manufacturing alumina-based ceramics and some other ceramics with high strength, low shrinkage and high quality.     

Fabrication of ceramic membranes on porous ceramic supports by electrophoretic deposition

Abstract

Nanoporous alumina membrane and continuous zeolite L membrane were fabricated on the inner surface of microporous alumina tubes. In the former case, an electrophoretic deposition (EPD) technique was used for the deposition of bimodal alumina particles for the subsequent low temperature sintering. In the latter case, the EPD was used for the seeding process of zeolite L particles for the subsequent hydrothermal synthesis. A thin layer of polypyrrole was synthesised on the inside wall of the porous tubes by the chemical polymerisation of pyrrole to give the wall electric conduction for the EPD electrode. The thickness of the coating layers was controlled by altering the applied voltage and deposition time. The interfacial connection of the alumina or zeolite coated layer and the substrate was evaluated by SEM observations before and after the thermal treatment. The nanoporous structure of the alumina membrane was also characterised by a pore size analyser.     

Process development for the laser powder bed fusion of WC-Ni Cermets using sintered-agglomerated powder

Although ceramic particle-metal matrix materials (i.e., cermets) can offer superior performance, manufacturing these materials via conventional means is difficult compared to the manufacturing of metal alloys. This study leverages the laser powder bed fusion (LPBF) process to additively manufacture dense tungsten carbide (WC)-17 wt.% nickel (Ni) composite specimens using novel spherical, sintered-agglomerated composite powder. A range of processing parameters yielding high-density specimens was discovered using a sequential series of experiments comprised of single bead, multi-layer, and cylindrical builds. Cylinders with a relative density >99% were fabricated and characterized in terms of microstructure, chemical composition, and hardness. Scanning electron microscopy images show favorable wetting between the Ni binder and carbide particles without any phase segregation and laser processing increased the average carbide particle size. Energy dispersive X-ray and X-ray diffraction analyses detected traces of secondary products after laser processing. For samples processed at high energy densities, complex carbides and carbon agglomerate phases were detected. The maximum hardness of 60.38 Rockwell C is achieved in the printed samples. The successful builds in this study open the way for LPBF of dense WC-Ni parts with a large workable laser power-laser velocity processing window.     

Effects of B4C addition on the microstructure and properties of porous alumina ceramics fabricated by direct selective laser sintering

Direct selective laser sintering (dSLS) is a promising method for the fabrication of complex-shaped ceramic parts. In this paper, boron carbide (B₄C) was used as an inorganic additive to improve the laser sintering behavior of alumina. The effects of B₄C addition on the microstructure and mechanical properties of porous alumina ceramics were investigated. Mixture of alumina powders and different amount of B₄C were directly sintered using different SLS parameters. Results indicated that the process window of alumina could be expanded by the addition of B₄C. Furthermore, the amount of B₄C played an important role in surface morphologies of alumina ceramics. It could be explained by the increase of mass transfer due to the addition of B₄C, which enhanced the densification process. The compressive strength of sintered samples increased with the increase of B₄C, which reached its maximum value when the content of B₄C was 7?wt% and the density of the samples after post treatment could reach 1.4?g/cm³. In addition, a size expansion phenomenon was observed. The size expansion could reach 5% after SLS, which could be attributed to the pin effects and oxidation behavior of B₄C particles.     

Dual-scale porous biphasic calcium phosphate gyroid scaffolds using ceramic suspensions containing polymer microsphere porogen for digital light processing

This study demonstrates a novel type of biphasic calcium phosphate (BCP) gyroid scaffolds featuring of gyroid macroporous structure and micropous BCP walls using poly(methyl methacrylate) (PMMA) microspheres as the porogen for ceramic digital light processing (DLP) technique. To tailor the microporosity of the BCP walls and the overall porosity of the dual-scale porous BCP scaffolds, the PMMA content with regard to the BCP powder was controlled in the range of 40 vol% to 70 vol%. After debinding at 600 °C and sintering at 1200 °C for 3 h, micropores were uniformly created throughout each BCP framework, while preserving 3?dimensional gyroid macroporous structures. As the PMMA content increased from 40 vol% to 70 vol%, the microporosity remarkably increased from 31.9 (±2.5) vol% to 55.2 (±1.4) vol%. This approach allowed the achievement of very high overall porosities (82.2–89.7 vol%) for the dual-scale porous scaffolds. However, all the scaffolds showed reasonable compressive strengths (0.8 MPa ?2.1 MPa), which are comparable to those of cancellous bones.     

Nanostructured materials prepared by use of ordered porous alumina membranes

We report on three different methods to prepare nanostructured materials using highly ordered porous alumina membranes as templates: (1) firstly, a new and simple method, termed as the paired cell method, was developed for the preparation of inorganic nanowires. Several kinds of inorganic nanowires were synthesized using this method. The structure and composition of these nanowires were determined by field emission scanning electron microscopy, transmission electron microscopy and energy dispersive X-ray spectroscopy. (2) Secondly, highly ordered platinum nanowire arrays were prepared by electrochemical method with the help of porous alumina membrane templates. The structure and composition of these nanowire arrays were also characterized by various experimental techniques. The electrochemically active surface area of the nanowire arrays was determined by cyclic voltammetry based on hydrogen adsorption. Results showed that the platinum nanowire arrays exhibited a large surface area. (3) Finally, we also present a simple and reliable procedure for the preparation of highly ordered metal nanohole and nanopillar arrays, based on the anodic oxidation of aluminum and vacuum evaporation technology. The field emission scanning electron microscopic images revealed that these metal nanostructure arrays were highly ordered over a large area. The nanoimprinting of aluminum surfaces using the as-prepared chromium nanopillar arrays was demonstrated, resulting in periodic indentation on the aluminum surface.     

Influence of resin composition on rheology and polymerization kinetics of alumina ceramic suspensions for digital light processing (DLP) additive manufacturing

Alumina ceramics with optimized microstructures and mechanical properties were obtained by the attractive digital lighting processing (DLP) additive manufacturing methodology in the present study. A acrylate-based resin system was designed for the alumina powders with a mean particle size of 0.5 μm. The influence of oligomer on the viscosity and polymerization kinetics of the ceramic suspensions has been elaborately discussed by rheology, curing depth and photo-DSC characterizations. The results indicated that the introduction of oligomer has improved the cross-linking density of resins and decreased the critical dose of energy for resin polymerization, which contributed to a tougher ceramic-resin slice with higher dimensional accuracy. Densifying processes including debinding and high temperature sintering of the ceramic parts were conducted according to the TG-DTA characterizations, alumina ceramics with uniform microstructures and eliminated delamination or intralaminar cracks were finally obtained. The flexural strength was 471 MPa for the ceramics obtained from the resin composition containing 20 wt% oligomer, Weibull modulus for the ceramics were determined to be 17.31 by evaluating thirty all sides polished ceramics, indicating the highly uniform property of the ceramics fabricated by DLP additive manufacturing.     

Micromachining porous alumina ceramic for high quality trimming of turbine blade cores via double femtosecond laser scanning

Turbine blade cores are made of porous alumina ceramic and determine the molding accuracy of the cavity of turbine blades, which strongly affect thermal diffusion performance and service life of turbine engines. To get a high quality ceramic core, accurate trimming for a preliminarily processed core is needed and therefore, micromachining porous alumina ceramic, which differs from general alumina substrates, is crucial. This paper dealt with a processing technology for the special material via double femtosecond laser scanning. The materials ablation threshold was firstly determined through parameter fitting and then this material was machined at a combination of different laser processing parameters. Considering the produced debris blocks the lasers further propagation into the material, double femtosecond laser scanning was newly proposed and experimentally verified with the comparison of gas jet assist and underwater laser processing ways. The removal profiles of the machined material were characterized in terms of cutting width, cutting depth, deviation of linearity and surface morphology, which exhibited high dependence on the femtosecond laser processing parameters. The optimal laser operating window was identified and high quality laser cutting of the porous alumina ceramic was demonstrated. The developed processing technology has potential application in trimming for ceramic casting cores. In addition, it might also give a novel view for high quality laser micromachining another materials.     

Strengthened porous alumina membrane tube prepared by means of internal anodic oxidation

A method for preparing an anodic aluminum oxide tube with a much higher mechanical strength than before was developed, where anodic oxidation was carried out from the inside of an aluminum tube (internal anodizing method). It was considered that the internal stress remaining in the alumina layer, which was formed in the course of the internal anodizing, resulted in a considerable improvement of compressive strength against external pressure. As a matter of fact, the tube could withstand at least up to 0.98 MPa of transmembrane pressure, which corresponded to 32.6 MPa in terms of breaking pressure. The tubular alumina membrane obtained had straight mesopores of 20–25 nm in diameter and, therefore, showed the Knudsen permselectivity for inorganic gases. Such a strengthened alumina tube is expected to be used as a porous membrane or as a support for composite membranes.     

添加锰矿粉和碳酸钙对铝硅质陶粒支撑剂材料性能的影响

以二级铝矾土生料、黏土为原料,以锰矿粉和碳酸钙为烧结剂,制备了高强度陶粒支撑剂材料,并讨论了锰矿粉加入量(w)0、1.0%、3.0%、5.0%、7.0%和碳酸钙加入量(w)0.5%、1.0%、1.5%、2.0%以及热处理温度为1 280、1 320、1 360、1 400℃时对支撑剂材料性能的影响。结果表明:随锰矿粉加入量的增加,试样烧结致密度提高,强度增大,当锰矿粉加入量≥5.0%(w)时,试样的强度基本不变;在加入5.0%(w)锰矿粉基础上,添加碳酸钙,试样烧后强度随碳酸钙加入量的提高而提高;碳酸钙加入量为2.0%(w)时,试样的强度达到275 MPa;同时添加5.0%(w)锰矿粉和2.0%(w)碳酸钙的试样的较佳热处理温度为1 360℃。     

超增溶自组装制备纳米氧化铝渣油加氢催化剂载体

采用超增溶胶团自组装体原位合成纳米微粒方法合成了氧化铝渣油加氢催化剂载体,并通过扫描电镜、吸附脱附BET法和热重分析表征其结构。结果表明,制备的超增溶纳米自组装氧化铝载体性能稳定,分布均匀,具有较大的孔径、比表面积和孔容,强度高,堆积密度小,符合纳米粒子特性。